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CROSS REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. application Ser. No. 12/058,417 filed on Mar. 28, 2008, and claims priority to Korean Patent Application No. 10-2007-0032018, filed Mar. 30, 2007, which are all hereby incorporated by reference for all purposes as if fully set forth herein.
FIELD OF THE INVENTION
The present invention relates to a light emitting diode (LED) package, and more particularly, to an LED package with a metal PCB.
BACKGROUND OF THE INVENTION
In general, an LED is an element in which electrons and holes are combined in a P-N semiconductor junction structure by application of current thereby emitting certain light. The LED is typically formed to have a package structure, in which an LED chip is mounted, and is frequently referred to as an “LED package.” Such an LED package is generally mounted on a printed circuit board (PCB) and receives current applied from electrodes formed on the PCB to thereby emit light.
In an LED package, heat generated from an LED chip has a direct influence on the light emitting performance and life span of the LED package. The reason is that when heat generated from the LED chip remains for a long period of time, dislocation and mismatch occur in a crystal structure of the LED chip. Moreover, a high power LED package has been recently developed. Since the high power LED package is operated by high-voltage power and a large amount of heat is generated in an LED chip due to the high voltage, a separate device for effectively dissipating the generated heat is required.
Therefore, there has been developed a conventional LED package for enhancing heat dissipation performance using a metal printed circuit board (metal PCB) in which an insulating layer and a metal pattern layer are sequentially formed on an aluminum base. For example, such a conventional LED package is fabricated in such a manner that a hole cup is formed in the aluminum base so that a portion of the aluminum base is exposed upward by a groove machining process such as cutting, an LED chip adheres to the hole cup, and then the LED chip and the metal pattern layer are connected to each other through a conductive wire.
However, the conventional LED package is difficult to be fabricated into a compact structure due to a large thickness of the aluminum base, and does not have a lead structure for electrically connecting the LED chip to external electrodes. For this reason, it may be difficult to mount the conventional LED package on a typically used PCB. This means that the conventional LED package is less compatible with a conventional electronic device or is illumination device. Since current LED package manufacturers mostly have equipments suitable for fabricating LED packages with a lead structure, the conventional LED package limits the use of the existent equipments as described above. For this reason, the conventional LED package is also uneconomical.
Additionally, in the conventional LED package, since the hole cup is formed by a groove machining process such as a cutting process, the mounting surface of an LED chip is uneven due to the groove machining process, which causes a die attaching process of an LED chip to be difficult. In addition, the die-attached LED chip may be easily damaged due to thermal and mechanical impact.
An object of the present invention is to provide an LED package having a metal PCB, which has a superior heat dissipation property and a compact structure, does not largely restrict use of conventional equipments, and is compatible with an electronic device or illumination device currently used widely.
An LED package according to an aspect of the present invention comprises a metal printed circuit board (PCB) formed by laminating first and second sheet metal plates with an electric insulating layer interposed therebetween; and an LED chip mounted on the first sheet metal plate of the metal PCB, wherein the first sheet metal plate has electrode patterns and leads respectively extending from the electrode patterns.
At this time, each of the leads is preferably formed by bending a portion of the first sheet metal plate extending in an outer side direction from the metal PCB. More preferably, each of the leads has an enlarged contact area with an external electrode through two-step bending of the portion of the first sheet metal plate. Accordingly, each lead can have an enlarged contact area with an external electrode.
Alternatively, each of the leads may comprises a terminal pattern formed by patterning the second sheet metal plate in correspondence to the electrode pattern; and a via conductive portion passing through the metal PCB to connect the electrode pattern and the terminal pattern.
According to preferred embodiments of the present invention, the first and second sheet metal plates may be made of copper or copper alloy. The LED package may further comprise a molding member formed on the first sheet metal plate to cover the LED chip. The LED package may further comprise a hole cup formed around the LED chip to adjust a directional angle of light emitted from the LED chip. The hole cup may be formed of resin, metal, ceramic or a composite thereof. The hole cup may be made of an FR4 material. Further, the hole cup may include an insulating plate and a metal reflective plate, each of which has an opening, and which are sequentially formed on the first sheet metal plate. In addition, the metal reflective plate may be made of aluminum.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view showing an LED package according to an embodiment of the present invention;
FIG. 2 is a sectional view of the LED package shown in FIG. 1 ;
FIG. 3 is a view illustrating an example of manufacturing a plurality of LED packages having one large metal PCB as a base; and
FIG. 4 is a sectional view of an LED package according to another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
FIG. 1 is a perspective view showing an LED package according to an embodiment of the present invention, and FIG. 2 is a sectional view of the LED package shown in FIG. 1 .
As shown in FIGS. 1 and 2 , the LED package 1 of this embodiment comprises a metal PCB 10 , an LED chip 2 mounted on the metal PCB 10 , and the like. A transparent molding member 31 for protecting the LED chip 2 is formed on the metal PCB 10 in a generally hemispherical shape. The molding member 31 further includes an extension portion 32 extending integrally with the molding member 31 to cover portions of top and side surfaces of the metal PCB 10 , and the extension portion 32 can protect not only the LED chip 2 but also the metal PCB 10 from the outside.
The metal PCB 10 of this embodiment comprises first and second sheet metal plates 16 and 12 and an insulating layer 14 interposed between the sheet metal plates 16 and 12 , wherein the first and second sheet metal plates 16 and 12 are laminated with the insulating layer 14 interposed therebetween. The second sheet metal plate 12 is made of copper or copper alloy to form a base of the metal PCB 10 , and the first sheet metal plate 16 is made of copper or copper alloy to be electrically insulated from the second sheet metal plate 12 by the insulating layer 14 .
The first sheet metal plate 16 comprises a first electrode pattern 162 a , to which the LED chip 2 adheres, and a second electrode pattern 162 b patterned to be spaced apart from the first electrode pattern 162 a . The LED chip 2 on the first electrode pattern 162 a is electrically connected to the second electrode pattern 162 b by a bonding wire W. At this time, the insulating layer 14 has an electrically insulating property. For the purpose of smooth dissipation of heat generated from the LED chip 2 , the insulating layer 14 is preferably formed of a material with excellent thermal conductivity.
According to the embodiment of the present invention, the first sheet metal plate 16 further includes leads 164 a and 164 b extending in an outer side direction of the metal PCB 10 . The leads 164 a and 164 b are portions connected to external electrodes on an external PCB (not shown) on which the LED package 1 is mounted. Through two-step bending, each of the leads 164 a and 164 b is directed downward and has a broad contact area with an external electrode (not shown). That is, each of the leads 164 a and 164 b is bent to be directed downward through a first bending process and to fold up through a second bending process, thereby having an end with a thickness greater than the original thickness of the first sheet metal plate 16 .
The LED package 1 shown in FIGS. 1 and 2 is of a top view type in which a package mounting surface and a light emitting surface are positioned to be opposite to each other due to the bending positions and directions of the leads 164 a and 164 b . However, it may be considered that the bending positions and directions of the leads 164 a and 164 b are different from each other whereby the package mounting surface and the light emitting surface are perpendicular to each other. As such, the configuration in which the package mounting surface and the light emitting surface are perpendicular to each other is suitable for implementing an LED package typically called a side view type LED package.
In addition, the LED package 1 of this embodiment further includes a hole cup 20 for obtaining a desired directional angle of light, i.e., for adjusting the directional angle of light emitted from the LED chip 2 . The hole cup 20 includes an opening, in which a portion of the molding member 31 is filled, and serves to reflect light within a desired directional angle range by surrounding a circumference of the LED chip 2 on the first sheet metal plate 16 . Since the hole cup 20 is directly laminated on the first sheet metal plate 16 of the metal PCB 10 , it is unnecessary to form the hole cup 20 by machining a groove in the metal PCB 10 . Accordingly, the chip mounting surface of the metal PCB 10 is formed to be flat unlike the prior art.
According to the embodiment of the present invention, the hole cup 20 may be used by forming an opening in a plate-shaped member and formed of a resin, metal, ceramic or a composite thereof. As an example, the hole cup 20 may be formed of a material such as FR4. The FR4 is Epoxy Resin Bonded Glass Fiber (ERBGF) reinforced by combining glass fiber with epoxy, which has excellent strength and light reflexibility, and is generally used as a raw material of PCBs.
As another example, the hole cup 20 may be formed in such manner that an insulating plate 21 and a metal reflective plate 22 , which are respectively formed with openings, adhere to each other as shown in the enlarged view of FIG. 2 . At this time, the insulating plate 21 serves to cause the metal reflective plate 22 and the first sheet metal plate 16 positioned under the insulating plate 21 to be electrically insulated. Preferably, the metal reflective plate 22 is made of an aluminum material.
According to the embodiment of the present invention, the aforementioned metal PCB 10 is a unit metal PCB cut and separated from a large metal PCB 10 ′ (hereinafter, referred to as a “laminated raw material”) shown in FIG. 3 , and a plurality of the LED packages 1 , each of which has the metal PCB 10 , are previously formed using the laminated raw material 10 ′ as a base, as shown in FIG. 3 . The laminated raw material 10 ′ is a laminate of the first sheet metal plate 16 , the insulating layer 14 and the second sheet metal plate 12 , which are patterned and machined to have a predetermined shape. The plurality of LED packages 1 are supported on the laminated raw material 10 ′ through the leads 164 a and 164 b extending from the first sheet metal plate 16 and supporting portions 102 ′ of the respective layers. The supporting portions 102 ′ and the leads 164 a and 164 b are cut, and the leads 164 a and 164 b are bent as described above, thereby completing the unit LED packages 1 each having the configuration shown in FIGS. 1 and 2 .
FIG. 4 is a sectional view of an LED package 1 according to another embodiment of the present invention. The LED package 1 of this embodiment has a configuration substantially equal to the aforementioned embodiment, except the configuration of leads extending from the electrode patterns 162 a and 162 b of the first sheet metal plate 16 . Hereinafter, the configuration of the leads different from those of the previous embodiment will be mainly described.
As shown in FIG. 4 , the leads of this embodiment include terminal patterns 121 and 122 formed by patterning a second sheet metal plate 12 in correspondence to electrode patterns 162 a and 162 b of a first sheet metal plate 16 , and via conductive portions 165 a and 165 b passing through a metal PCB 10 to connect the electrode patterns 162 a and 162 b and the terminal patterns 121 and 122 . At this time, the via conductive portions 165 a and 165 b may be formed by previously forming openings bored through the metal PCB 10 and then filling the openings with a metal made of the same material as the first sheet metal plate 16 and/or the second sheet metal plate 12 , for example, by a plating method or the like.
As described above, an LED package according to the present invention has a sufficient heat dissipation property and a compact structure, and includes leads connected to external electrodes while using a metal PCB and having a structure approximately equal to a general LED package, thereby having excellent compatibility with a conventional electronic device or illumination device. Further, the LED package according to the present invention and a general LED package without a metal PCB are manufactured through a considerably similar process. Thus, there is an economical advantage in that many equipments possessed by current LED package manufacturers can be used in manufacturing the LED package according to the present invention as they are. Furthermore, an additional groove machining process is not required to form a hole cup in which an LED chip is positioned, so that LED package according to the present invention has a flat chip mounting surface. Accordingly, a die attaching process of the LED chip can be performed more easily as compared with a conventional metal PCB-type LED package, and the die attached LED chip is strong against thermal and mechanical impact.
Although the present invention have been described with a specified embodiment, it will be apparent to those skilled in the art that various modifications, changes and variations can be made thereto within the scope of the present invention and the appended claims. Therefore, the aforementioned descriptions and the accompanying drawings should be construed as not limiting the technical spirit of the present invention but illustrating the present invention. | The present invention relates to a light emitting diode (LED) package. An object of the present invention is to provide an LED package having a metal PCB, which has a superior heat dissipation property and a compact structure, does not largely restrict use of conventional equipments, and is compatible with an electronic device or illumination device currently used widely. To this end, an LED package according to the present invention comprises a metal printed circuit board (PCB) formed by laminating first and second sheet metal plates with an electric insulating layer interposed therebetween; and an LED chip mounted on the first sheet metal plate of the metal PCB, wherein the first sheet metal plate has electrode patterns and leads respectively extending from the electrode patterns. | 7 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority from and the benefit of U.S. Provisional Application Ser. No. 60/867,043, entitled MICROCHANNEL HEAT EXCHANGER APPLICATIONS, filed Nov. 22, 2006, and U.S. Provisional Application Ser. No. 60/882,033, entitled MICROCHANNEL HEAT EXCHANGER APPLICATIONS, filed Dec. 27, 2006, which are hereby incorporated by reference.
BACKGROUND
[0002] The invention relates generally to multi-block circuit multichannel heat exchangers.
[0003] Heat exchangers are used in heating, ventilation, air conditioning, and refrigeration (HVAC&R) systems. Multichannel heat exchangers generally include multichannel tubes for flowing refrigerant through the heat exchanger. Each multichannel tube may contain several individual flow channels. Fins may be positioned between the tubes to facilitate heat transfer between refrigerant contained within the tube flow channels and external air passing over the tubes. Multichannel heat exchangers may be used in small tonnage systems, such as residential systems, or in large tonnage systems, such as industrial chiller systems.
[0004] In general, heat exchangers transfer heat by circulating a refrigerant through a cycle of evaporation and condensation. In some systems, one heat exchanger may contain multiple coil circuits for circulating two or more fluids in order to provide cooling or heating to different parts of a system. In other systems, one heat exchanger may contain multiple coil circuits for circulating the same fluid through the heat exchanger more than once in order to provide increased heating or cooling.
[0005] The location of a coil circuit within the heat exchanger may impact the rate of heat transfer because environmental conditions may vary depending on a tube's position within the heat exchanger. For example, in a heat exchanger containing horizontal tubes, the bottom tubes may receive less airflow than the top tubes, resulting in a lower rate of heat transfer between the bottom tubes and the environment. In a heat exchanger containing vertical tubes, the outer tubes may receive less airflow based on proximity to other equipment or an outer wall. In a multiple heat exchanger configuration, the outer heat exchanger coils may receive more airflow, resulting in a higher rate of heat transfer between these tubes and the environment.
[0006] Furthermore, the type of fluid within a coil circuit may be used to configure the location of the circuit within the heat exchanger slab. For example, it may be desirable to locate a condenser circuit containing a lower temperature fluid within a section of the heat exchanger that receives less airflow because less heat transfer is generally needed between the lower temperature fluid and the environment. In some applications, the lower temperature fluid may be a refrigerant requiring subcooling or an electrical coolant used to cool an electrical power circuit. Conversely, it may be desirable to locate a fluid undergoing a phase change in a section of the heat exchanger that receives more airflow.
SUMMARY
[0007] In accordance with aspects of the invention, a heat exchanger is presented that includes four groups of multichannel tubes disposed adjacent to one another. Group A is configured to receive a flow of a first fluid to be cooled or heated. Group B is configured to receive the flow of the first fluid from group A. Group C is configured to receive a flow of a second fluid to be cooled or heated. Group D is configured to receive the flow of the second fluid from group C.
[0008] In accordance with further aspects of the invention, a heat exchanger and a system including a heat exchanger are presented. The heat exchanger includes a first manifold, a second manifold, a first multi-pass circulating block in fluid communication with the manifolds, and a second multi-pass circulating block in fluid communication with the manifolds. The first block includes two groups, group A and group B, of multichannel tubes disposed adjacent to one another. Group A is configured to receive a flow of a first fluid to be cooled or heated, and group B is configured to receive the flow of the first fluid from group A. The second block includes two other groups, group C and group D, of multichannel tubes disposed adjacent to one another. Group C is configured to receive a flow of a second fluid to be cooled or heated, and group D is configured to receive the flow of the second fluid from group C.
DRAWINGS
[0009] FIG. 1 is a perspective view of an exemplary residential air conditioning or heat pump system of the type that might employ a heat exchanger
[0010] FIG. 2 is a partially exploded view of the outside unit of the system of FIG. 1 , with an upper assembly lifted to expose certain of the system components, including a heat exchanger.
[0011] FIG. 3 is a perspective view an illustration of an exemplary commercial or industrial HVAC&R system that employs a chiller and air handlers to cool a building and that may also employ heat exchangers.
[0012] FIG. 4 is a diagrammatical overview of an exemplary air conditioning system which may employ one or more heat exchangers containing coil circuits.
[0013] FIG. 5 is a diagrammatical overview of an exemplary heat pump system which may employ one or more heat exchangers containing coil circuits.
[0014] FIG. 6 is a perspective view of an exemplary heat exchanger illustrating coil circuiting positions.
[0015] FIG. 7 is a detail perspective view of the heat exchanger of FIG. 6 sectioned through the multichannel tubes.
[0016] FIG. 8 is a perspective view of exemplary heat exchanger illustrating an alternate coil circuiting positions.
[0017] FIG. 9 is a perspective view of exemplary heat exchanger illustrating another alternate coil circuiting position.
[0018] FIG. 10 is a detail perspective of the manifold employed in the coil circuiting position illustrated in FIG. 9 .
DETAILED DESCRIPTION
[0019] FIGS. 1-3 depict exemplary applications for heat exchangers. Such systems, in general, may be applied in a range of settings, both within the HVAC&R field and outside of that field. In presently contemplated applications, however, heat exchanges may be used in residential, commercial, light industrial, industrial and in any other application for heating or cooling a volume or enclosure, such as a residence, building, structure, and so forth. Moreover, the heat exchanges may be used in industrial applications, where appropriate, for basic refrigeration and heating of various fluids. FIG. 1 illustrates a residential heating and cooling system. In general, a residence, designated by the letter R, will be equipped with an outdoor unit OU that is operatively coupled to an indoor unit IU. The outdoor unit is typically situated adjacent to a side of the residence and is covered by a shroud to protect the system components and to prevent leaves and other contaminants from entering the unit. The indoor unit may be positioned in a utility room, an attic, a basement, and so forth. The outdoor unit is coupled to the indoor unit by refrigerant conduits RC that transfer primarily liquid refrigerant in one direction and primarily vaporized refrigerant in an opposite direction.
[0020] When the system shown in FIG. 1 is operating as an air conditioner, a coil in the outdoor unit serves as a condenser for recondensing vaporized refrigerant flowing from indoor unit IU to outdoor unit OU via one of the refrigerant conduits. In these applications, a coil of the indoor unit, designated by the reference characters IC, serves as an evaporator coil. The evaporator coil receives liquid refrigerant (which may be expanded by an expansion device described below) and evaporates the refrigerant before returning it to the outdoor unit.
[0021] The outdoor unit draws in environmental air through sides as indicated by the arrows directed to the sides of unit OU, forces the air through the outer unit coil by a means of a fan (not shown) and expels the air as indicated by the arrows above the outdoor unit. When operating as an air conditioner, the air is heated by the condenser coil within the outdoor unit and exits the top of the unit at a temperature higher than it entered the sides. Air is blown over indoor coil IC, and is then circulated through the residence by means of ductwork D, as indicated by the arrows in FIG. 1 . The overall system operates to maintain a desired temperature as set by a thermostat T. When the temperature sensed inside the residence is higher than the set point on the thermostat (plus a small amount), the air conditioner will become operative to refrigerate additional air for circulation through the residence. When the temperature reaches the set point (minus a small amount), the unit will stop the refrigeration cycle temporarily.
[0022] When the unit in FIG. 1 operates as a heat pump, the roles of the coils are simply reversed. That is, the coil of the outdoor unit will serve as an evaporator to evaporate refrigerant and thereby cool air entering the outdoor unit as the air passes over the outdoor unit coil. Indoor coil IC will receive a stream of air blown over it and will heat the air by condensing a refrigerant.
[0023] FIG. 2 illustrates a partially exploded view of one of the units shown in FIG. 1 , in this case outdoor unit OU. In general, the unit may be thought of as including an upper assembly UA made up of a shroud, a fan assembly, a fan drive motor, and so forth. In the illustration of FIG. 2 , the fan and fan drive motor are not visible because they are hidden by the surrounding shroud. An outdoor coil OC is housed within this shroud and is generally deposed to surround or at least partially surround other system components, such as a compressor, an expansion device, a control circuit.
[0024] FIG. 3 illustrates another exemplary application, in this case an HVAC&R system for building environmental management. A building BL is cooled by a system that includes a chiller CH, which is typically disposed on or near the building, or in an equipment room or basement. Chiller CH is an air-cooled device that implements a refrigeration cycle to cool water. The water is circulated to a building through water conduits WC. The water conduits are routed to air handlers AH at individual floors or sections of the building. The air handlers are also coupled to ductwork DU that is adapted to blow air from an outside intake OI.
[0025] Chiller CH, which includes heat exchangers for both evaporating and condensing a refrigerant as described above, cools water that is circulated to the air handlers. Air blown over additional coils that receive the water in the air handlers causes the water to increase in temperature and the circulated air to decrease in temperature. The cooled air is then routed to various locations in the building via additional ductwork. Ultimately, distribution of the air is routed to diffusers that deliver the cooled air to offices, apartments, hallways, and any other interior spaces within the building. In many applications, thermostats or other command devices (not shown in FIG. 3 ) will serve to control the flow of air through and from the individual air handlers and ductwork to maintain desired temperatures at various locations in the structure.
[0026] FIG. 4 illustrates an air conditioning system 10 , which uses heat exchangers containing multichannel tubes. Refrigerant flows through the system within closed refrigeration loop 12 . The refrigerant may be any fluid that absorbs and extracts heat. For example, the refrigerant may be hydrofluorocarbon (HFC) based R-410A, R-407, or R-134a, or it may be carbon dioxide (R-744a) or ammonia (R-717). Air conditioning system 10 includes control devices 14 that enable system 10 to cool an environment to a prescribed temperature.
[0027] System 10 cools an environment by cycling refrigerant within closed refrigeration loop 12 through condenser 16 , compressor 18 , expansion device 20 , and evaporator 22 . The refrigerant enters condenser 16 as a high pressure and temperature vapor and flows through the multichannel tubes of condenser 16 . A fan 24 , which is driven by a motor 26 , draws air across the multichannel tubes. Fan 24 may push or pull air across the tubes. Heat transfers from the refrigerant vapor to the air producing heated air 28 and causing the refrigerant vapor to condense into a liquid. The liquid refrigerant then flows into an expansion device 20 where the refrigerant expands to become a low pressure and temperature liquid. Typically, expansion device 20 will be a thermal expansion valve (TXV); however, in other embodiments, the expansion device may be an orifice or a capillary tube. After the refrigerant exits the expansion device, some vapor refrigerant may be present in addition to the liquid refrigerant.
[0028] From expansion device 20 , the refrigerant enters evaporator 22 and flows through the evaporator multichannel tubes. A fan 30 , which is driven by a motor 32 , draws air across the multichannel tubes. Heat transfers from the air to the refrigerant liquid producing cooled air 34 and causing the refrigerant liquid to boil into a vapor. In some embodiments, the fan may be replaced by a pump that draws fluid across the multichannel tubes.
[0029] The refrigerant then flows to compressor 18 as a low pressure and temperature vapor. Compressor 18 reduces the volume available for the refrigerant vapor, consequently, increasing the pressure and temperature of the vapor refrigerant. The compressor may be any suitable compressor such as a screw compressor, reciprocating compressor, rotary compressor, swing link compressor, scroll compressor, or turbine compressor. Compressor 18 is driven by a motor 36 that receives power from a variable speed drive (VSD) or a direct AC or DC power source. In one embodiment, motor 36 receives fixed line voltage and frequency from an AC power source although in some applications the motor may be driven by a variable voltage or frequency drive. The motor may be a switched reluctance (SR) motor, an induction motor, an electronically commutated permanent magnet motor (ECM), or any other suitable motor type. The refrigerant exits compressor 18 as a high temperature and pressure vapor that is ready to enter the condenser and begin the refrigeration cycle again.
[0030] The operation of the refrigeration cycle is governed by control devices 14 that include control circuitry 38 , an input device 40 , and a temperature sensor 42 . Control circuitry 38 is coupled to motors 26 , 32 , and 36 that drive condenser fan 24 , evaporator fan 30 , and compressor 18 , respectively. The control circuitry uses information received from input device 40 and sensor 42 to determine when to operate motors 26 , 32 , and 36 that drive the air conditioning system. In some applications, the input device may be a conventional thermostat. However, the input device is not limited to thermostats, and more generally, any source of a fixed or changing set point may be employed. These may include local or remote command devices, computer systems and processors, and mechanical, electrical, and electromechanical devices that manually or automatically set a temperature-related signal that the system receives. For example, in a residential air conditioning system, the input device may be a programmable 24-volt thermostat that provides a temperature set point to the control circuitry. Sensor 42 determines the ambient air temperature and provides the temperature to control circuitry 38 . Control circuitry 38 then compares the temperature received from the sensor to the temperature set point received from the input device. If the temperature is higher than the set point, control circuitry 38 may turn on motors 26 , 32 , and 36 to run air conditioning system 10 . The control circuitry may execute hardware or software control algorithms to regulate the air conditioning system. In some embodiments, the control circuitry may include an analog to digital (A/D) converter, a microprocessor, a non-volatile memory, and an interface board. Other devices may, of course, be included in the system, such as additional pressure and/or temperature transducers or switches that sense temperatures and pressures of the refrigerant, the heat exchangers, the inlet and outlet air, and so forth.
[0031] FIG. 5 illustrates a heat pump system 44 that uses multichannel tubes. Because the heat pump may be used for both heating and cooling, refrigerant flows through a reversible refrigeration/heating loop 46 . The refrigerant may be any fluid that absorbs and extracts heat. The heating and cooling operations are regulated by control devices 48 .
[0032] Heat pump system 44 includes an outside coil 50 and an inside coil 52 that both operate as heat exchangers. The coils may function either as an evaporator or as a condenser depending on the heat pump operation mode. For example, when heat pump system 44 is operating in cooling (or “AC”) mode, outside coil 50 functions as a condenser, releasing heat to the outside air, while inside coil 52 functions as an evaporator, absorbing heat from the inside air. When heat pump system 44 is operating in heating mode, outside coil 50 functions as an evaporator, absorbing heat from the outside air, while inside coil 52 functions as a condenser, releasing heat to the inside air. A reversing valve 54 is positioned on reversible loop 46 between the coils to control the direction of refrigerant flow and thereby to switch the heat pump between heating mode and cooling mode.
[0033] Heat pump system 44 also includes two metering devices 56 and 58 for decreasing the pressure and temperature of the refrigerant before it enters the evaporator. The metering device also acts to regulate refrigerant flow into the evaporator so that the amount of refrigerant entering the evaporator equals the amount of refrigerant exiting the evaporator. The metering device used depends on the heat pump operation mode. For example, when heat pump system 44 is operating in cooling mode, refrigerant bypasses metering device 56 and flows through metering device 58 before entering the inside coil 52 , which acts as an evaporator. In another example, when heat pump system 44 is operating in heating mode, refrigerant bypasses metering device 58 and flows through metering device 56 before entering outside coil 50 , which acts as an evaporator. In other embodiments, a single metering device may be used for both heating mode and cooling mode. The metering devices typically are thermal expansion valves (TXV), but also may be orifices or capillary tubes.
[0034] The refrigerant enters the evaporator, which is outside coil 50 in heating mode and inside coil 52 in cooling mode, as a low temperature and pressure liquid. Some vapor refrigerant also may be present as a result of the expansion process that occurs in metering device 56 or 58 . The refrigerant flows through multichannel tubes in the evaporator and absorbs heat from the air changing the refrigerant into a vapor. In cooling mode, the indoor air passing over the multichannel tubes also may be dehumidified. The moisture from the air may condense on the outer surface of the multichannel tubes and consequently be removed from the air.
[0035] After exiting the evaporator, the refrigerant passes through reversing valve 54 and into compressor 60 . Compressor 60 decreases the volume of the refrigerant vapor, thereby, increasing the temperature and pressure of the vapor. The compressor may be any suitable compressor such as a screw compressor, reciprocating compressor, rotary compressor, swing link compressor, scroll compressor, or turbine compressor.
[0036] From the compressor, the increased temperature and pressure vapor refrigerant flows into a condenser, the location of which is determined by the heat pump mode. In cooling mode, the refrigerant flows into outside coil 50 (acting as a condenser). A fan 62 , which is powered by a motor 64 , draws air over the multichannel tubes containing refrigerant vapor. In some embodiments, the fan may be replaced by a pump that draws fluid across the multichannel tubes. The heat from the refrigerant is transferred to the outside air causing the refrigerant to condense into a liquid. In heating mode, the refrigerant flows into inside coil 52 (acting as a condenser). A fan 66 , which is powered by a motor 68 , draws air over the multichannel tubes containing refrigerant vapor. The heat from the refrigerant is transferred to the inside air causing the refrigerant to condense into a liquid.
[0037] After exiting the condenser, the refrigerant flows through the metering device ( 56 in heating mode and 58 in cooling mode) and returns to the evaporator (outside coil 50 in heating mode and inside coil 52 in cooling mode) where the process begins again.
[0038] In both heating and cooling modes, a motor 70 drives compressor 60 and circulates refrigerant through reversible refrigeration/heating loop 46 . The motor may receive power either directly from an AC or DC power source or from a variable speed drive (VSD). The motor may be a switched reluctance (SR) motor, an induction motor, an electronically commutated permanent magnet motor (ECM), or any other suitable motor type.
[0039] The operation of motor 70 is controlled by control circuitry 72 . Control circuitry 72 receives information from an input device 74 and sensors 76 , 78 , and 80 and uses the information to control the operation of heat pump system 44 in both cooling mode and heating mode. For example, in cooling mode, input device 74 provides a temperature set point to control circuitry 72 . Sensor 80 measures the ambient indoor air temperature and provides it to control circuitry 72 . Control circuitry 72 then compares the air temperature to the temperature set point and engages compressor motor 70 and fan motors 64 and 68 to run the cooling system if the air temperature is above the temperature set point. In heating mode, control circuitry 72 compares the air temperature from sensor 80 to the temperature set point from input device 74 and engages motors 64 , 68 , and 70 to run the heating system if the air temperature is below the temperature set point.
[0040] Control circuitry 72 also uses information received from input device 74 to switch heat pump system 44 between heating mode and cooling mode. For example, if input device 74 is set to cooling mode, control circuitry 72 will send a signal to a solenoid 82 to place reversing valve 54 in air conditioning position 84 . Consequently, the refrigerant will flow through reversible loop 46 as follows: the refrigerant exits compressor 60 , is condensed in outside coil 50 , is expanded by metering device 58 , and is evaporated by inside coil 52 . If the input device is set to heating mode, control circuitry 72 will send a signal to solenoid 82 to place reversing valve 54 in heat pump position 86 . Consequently, the refrigerant will flow through the reversible loop 46 as follows: the refrigerant exits compressor 60 , is condensed in inside coil 52 , is expanded by metering device 56 , and is evaporated by outside coil 50 .
[0041] The control circuitry may execute hardware or software control algorithms to regulate the heat pump system 44 . In some embodiments, the control circuitry may include an analog to digital (A/D) converter, a microprocessor, a non-volatile memory, and an interface board.
[0042] The control circuitry also may initiate a defrost cycle when the system is operating in heating mode. When the outdoor temperature approaches freezing, moisture in the outside air that is directed over outside coil 50 may condense and freeze on the coil. Sensor 76 measures the outside air temperature, and sensor 78 measures the temperature of outside coil 50 . These sensors provide the temperature information to the control circuitry which determines when to initiate a defrost cycle. For example, if either of sensors 76 or 78 provides a temperature below freezing to the control circuitry, system 44 may be placed in defrost mode. In defrost mode, solenoid 82 is actuated to place reversing valve 54 in air conditioning position 84 , and motor 64 is shut off to discontinue air flow over the multichannels. System 44 then operates in cooling mode until the increased temperature and pressure refrigerant flowing through outside coil 50 defrosts the coil. Once sensor 78 detects that coil 50 is defrosted, control circuitry 72 returns the reversing valve 54 to heat pump position 86 . As will be appreciated by those skilled in the art, the defrost cycle can be set to occur at many different time and temperature combinations.
[0043] FIG. 6 is a perspective view of an exemplary heat exchanger 88 that may be used in air conditioning system 10 or heat pump system 44 . The exemplary heat exchanger may be a condenser 16 , an evaporator 22 , an outside coil 50 , or an inside coil 52 , as shown in FIGS. 4 and 5 . It should also be noted that in similar or other systems, the heat exchanger may be used as part of a chiller or in any other heat exchanging application. Heat exchanger 88 includes a top manifold 90 and a bottom manifold 92 , which are connected by multichannel tubes 94 . Although sixty tubes are shown in FIG. 6 , the number of tubes may vary. The manifolds and tubes may be constructed of aluminum or any other material that promotes good heat transfer. Refrigerant flows vertically within multichannel tubes 94 between manifolds 90 and 92 . In some embodiments, the heat exchanger may be rotated approximately 90 degrees so the multichannel tubes run horizontally between a left manifold and a right manifold. The heat exchanger may be inclined at an angle relative to the vertical axis. Furthermore, although the multichannel tubes are depicted as having an oblong shape, the tubes may be any shape, such as tubes with a cross-section in the form of a rectangle, square, circle, oval, ellipse, triangle, trapezoid, or parallelogram. In some embodiments, the tubes may have a diameter ranging from 0.5 mm to 3 mm. It should also be noted that the heat exchanger may be provided in a single plane or slab, or may include bends, corners, contours, and so forth.
[0044] Fins 96 are located between the multichannel tubes 94 to promote the transfer of heat between the tubes 94 and the environment. In one embodiment, the fins are constructed of aluminum, brazed or otherwise joined to the tubes, and disposed generally perpendicular to the flow of refrigerant. However, in other embodiments the fins may be made of other materials that facilitate heat transfer and may extend parallel or at varying angles with respect to the flow of the refrigerant. The fins may be louvered fins, corrugated fins, or any other suitable type of fin.
[0045] Baffles 98 , 100 , 102 , and 104 separate the multichannel tubes 94 into two coil circuits containing four groups of tubes. The four groups of tubes are disposed adjacent to one another to form a single slab heat exchanger 88 . Each individual group of tubes contains several tubes disposed adjacent to one another. The baffles direct the flow of refrigerant between manifolds 90 and 92 . Baffles 98 , 100 , and 102 divide top manifold 90 into four separate sections corresponding to the four groups of tubes, while baffle 104 divides bottom manifold 92 into two separate sections corresponding to two coil circuits. The baffles may be composed of any material which acts as a barrier to the flow of refrigerant. For example, in some embodiments, the baffles may be made from aluminum. In other embodiments, the baffles may be made from material having a low thermal conductivity in order to provide insulation between the groups of the tubes and the coil circuits.
[0046] Baffles 98 and 100 divide top manifold 90 into a tube group A 106 and a tube group B 108 . Baffle 100 directs the flow of refrigerant from top manifold 90 down to bottom manifold 92 through the multichannel tubes of group A 106 . The fluid then returns to the top manifold 90 through the multichannel tubes of group B 108 . Baffle 98 prevents the fluid that has returned to top manifold 90 from entering the tubes of tube group C 110 .
[0047] Baffles 98 and 102 divide top manifold 90 into a tube group C 110 and a tube group D 112 . Baffle 102 directs the flow of refrigerant from top manifold 90 down to bottom manifold 92 through the multichannel tubes of group C 110 . The refrigerant then returns to top manifold 90 through the multichannel tubes of group D 112 .
[0048] Baffles 98 and 104 divide the heat exchanger into two independent coil circuits. Baffle 98 divides top manifold 90 in order to prevent the fluid flowing within tube group B 108 from contacting the fluid flowing within tube group C 110 . Baffle 104 divides bottom manifold 92 to prevent the fluid flowing within tube group B 108 from contacting the fluid flowing within tube group C 110 . Consequently, the refrigerant that flows within the tubes of group A and group B does not contact the refrigerant that flows within the tubes of group C and group D.
[0049] Each independent coil circuit has its own inlet and outlet. The first coil circuit containing multichannel tubes of group A 106 and group B 108 includes inlet 114 and outlet 116 . Consequently, the refrigerant flows through the first coil circuit as follows: the refrigerant enters top manifold 90 through inlet 114 , flows through the group A 106 multichannel tubes to bottom manifold 92 , returns to top manifold 90 through the group B 108 multichannel tubes, and exits the heat exchanger through outlet 116 . Baffle 100 directs the flow of refrigerant from top manifold 90 to bottom manifold 92 while baffles 98 and 104 separate the first coil circuit from the second coil circuit.
[0050] The second coil circuit containing multichannel tubes of group C 110 and group D 112 has an inlet 118 and an outlet 120 . Consequently, the refrigerant flows through the second coil circuit as follows: the refrigerant enters the top manifold 90 through inlet 118 , flows through the group C 110 multichannel tubes to bottom manifold 92 , returns to top manifold 90 through the group D 112 multichannel tubes, and exits the heat exchanger through outlet 120 . Baffle 102 directs the flow of refrigerant from top manifold 90 to bottom manifold 92 while baffles 98 and 104 separate the second coil circuit from the first coil circuit.
[0051] The fluid that flows through the first coil circuit containing group A and B tubes may be the same type of fluid or different type of fluid than the fluid that flows through the second coil circuit containing group C and D tubes. In some embodiments, the fluid flowing through the first coil circuit may be the same fluid that flows through the second coil circuit, only at different stages in the heating and cooling process. For example, the second coil circuit may be used to provide a second pass for heating and cooling of the refrigerant. In other embodiments, the fluid flowing through the second coil circuit may be an independent fluid used to cool a separate part of the system such as a compressor or an electronic power circuit.
[0052] The number of tubes within each group may vary. For example, tube group A and tube group B may contain twenty tubes each while tube group C and tube group D contain thirty tubes each. In another example, tube group A may contain twenty tubes while tube group B contains fifteen tubes. Variations in the number of tubes may be used to improve heat transfer in each tube group by accounting for factors such as the phase of the refrigerant and the tube group location within the heat exchanger.
[0053] In other embodiments, the heat exchanger may be inclined at an angle or rotated 90 degrees so the fluid flows horizontally through the multichannel tubes instead of vertically. In the rotated embodiment, the manifolds may be positioned vertically on the sides of the heat exchanger. The coil circuiting concepts shown in FIG. 6 , as well as those shown in FIGS. 8 and 9 , may be used in other coil geometries, such as coils having an S-shape or an angled configuration. Furthermore, the coil circuiting concepts shown in FIGS. 6-9 may be repeated within a condenser slab to form a heat exchanger with more than four tube groups.
[0054] FIG. 7 depicts the heat exchanger of FIG. 6 sectioned through the multichannel tubes 94 to illustrate the internal configuration of the tubes. Refrigerant flows through flow channels 122 contained within tubes 94 . The direction of fluid flow 124 is from manifold 92 , shown in FIG. 6 , to manifold 90 . For example, as shown in FIG. 6 , tubes 94 of FIG. 7 may correspond to tubes from either group B or group D. The fluid flows through adjacent flow channels 122 in a relatively parallel flow between the manifolds. Flow channels 122 have a round cross-section with a small diameter relative to the size of the tubes 94 . In other embodiments, the flow channels may have a different cross-section such as that of a rectangular or oval shape. The cross-section and size of the flow channels may vary between the different tube groups.
[0055] FIG. 8 depicts an alternate coil circuiting configuration for the heat exchanger 88 . Note that the multichannel tubes and fins have been omitted for clarity. In this embodiment, tube group C 110 and tube group D 112 are located in between tube group A 106 and tube group B 108 . Fluid enters the multichannel tubes of group A 106 through inlet 114 and flows to bottom manifold 92 . The fluid flows across bottom manifold 92 to the multichannel tubes of group B 108 where it returns to the top manifold 90 and exits outlet 120 . Baffles 125 divide top manifold 90 into the four tube groups. Bottom manifold 92 , on the other hand, has a bypass 126 instead of a baffle. A second fluid enters the inlet 118 and flows through the tubes of group C 110 to the bypass 126 located within bottom manifold 92 . The bypass 126 may be constructed of any material sufficient for separating the fluids. The fluid flows through the bypass to the tubes of group D 112 which return it to the top manifold 90 where it exits through outlet 116 .
[0056] FIG. 9 depicts another alternate coil circuiting configuration for the heat exchanger 88 . Note that the multichannel tubes and fins have been omitted for clarity. In this embodiment, the tube groups A 106 and B 108 of the first coil circuit are alternated between the tube groups C 110 and D 112 of the second coil circuit. The top manifold 90 contains baffles 125 that divide it into the four tube groups, while the bottom manifold 92 contains a bypass 128 . Fluid enters the multichannel tubes of group A 106 through inlet 114 and flows to bottom manifold 92 where it enters a bypass 128 . Bypass 128 may be constructed of any material sufficient for separating fluids, such as aluminum. The fluid flows through the bypass to the multichannel tubes of group B 108 where it returns to top manifold 90 and exits through outlet 120 . A second refrigerant enters inlet 118 and flows through the tubes of group C 110 to bottom manifold 92 . The fluid flows through bottom manifold 92 to the tubes of group D 112 which return it to top manifold 90 where it exits through outlet 116 .
[0057] FIG. 10 shows manifold 90 configured for the coil circuiting shown in FIG. 9 . The cross-sectional view illustrates bypass 128 contained within manifold 90 . Bypass 128 divides the manifold into two flow sections, an outer flow section 130 and an inner flow section 132 . Fluid from group A, shown in FIG. 9 , flows through bypass 128 within inner flow section 132 to group B, shown in FIG. 9 . Fluid from group C, shown in FIG. 9 , flows through outer section 130 of the manifold to group D, shown in FIG. 9 . The outer flow exits the manifold to enter group D through an opening 134 . A similar inlet (not shown) directs the inner flow from the bypass into group B.
[0058] The coil circuiting configurations described herein may find application in a variety of heat exchangers and HVAC&R systems containing heat exchangers. However, the configurations are particularly well-suited to heat exchangers functioning as evaporators and condensers within chillers, air conditioners, and heat pumps. The coil circuiting configurations are intended to improve the overall efficiency of a heat exchanger by allowing tube groups to be positioned in a location of a heat exchanger that is tailored to the heat transfer properties of the tube group.
[0059] It should be noted that the present discussion makes use of the term “multichannel” tubes or “multichannel heat exchanger” to refer to arrangements in which heat transfer tubes include a plurality of flow paths between manifolds that distribute flow to and collect flow from the tubes. A number of other terms may be used in the art for similar arrangements. Such alternative terms might include “microchannel” and “microport.” The term “microchannel” sometimes carries the connotation of tubes having fluid passages on the order of a micrometer and less. However, in the present context such terms are not intended to have any particular higher or lower dimensional threshold. Rather, the term “multichannel” used to describe and claim embodiments herein is intended to cover all such sizes. Other terms sometimes used in the art include “parallel flow” and “brazed aluminum.” However, all such arrangements and structures are intended to be included within the scope of the term “multichannel.” In general, such “multichannel” tubes will include flow paths disposed along the width or in a plane of a generally flat, planar tube, although, again, the invention is not intended to be limited to any particular geometry unless otherwise specified in the appended claims.
[0060] While only certain features of the invention have been illustrated and described herein, many modifications and changes will occur to those skilled in the art. It is, therefore, to be understood that the appended claims are intended to cover all such modifications and changes as fall within the true spirit of the invention. Furthermore, in an effort to provide a concise description of the exemplary embodiments, all features of an actual implementation may not have been described. It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation specific decisions must be made. Such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure. | Heat exchangers containing various tube configurations and a heating, ventilation, air conditioning and refrigeration (HVAC&R) system employing these heat exchangers are provided which allow flexibility in directing fluids through a heat exchanger. Groups of tubes may be placed at different locations within a heat exchanger slab in order to tailor the heat transfer properties of each tube group to their location on the heat exchanger slab. Groups of tubes may be connected using manifolds to create coil circuits. | 5 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Continuation of U.S. application Ser. No. 11/974,704, filed Oct. 15, 2007, which is a Division of U.S. application Ser. No. 10/652,178, filed Aug. 29, 2003, the entire specifications of which are incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The invention relates to compositions and methods for removing copper from a surface. More particularly, it relates to removing copper residue from the barrel of a gun.
BACKGROUND OF THE INVENTION
[0003] When firearms, such as pistols, rifles and the like are fired, small amounts of residues deposit within the bore, that is, inside the barrel. This buildup is in fact a problem in nearly all kinds of guns, including very large bore armaments such as artillery pieces. The residues may include grease and other lubricants from bullets or cartridges, carbon from the burning of the propellant, and metallic deposits from the bullet. One particularly troublesome metallic deposit is copper, which is produced when copper-clad or brass-clad rounds of ammunition are fired. Over a period of time, copper and other deposits build up and adversely affect the efficiency and utility of the firearm. As a result, the firearm must be periodically cleaned to maintain maximum accuracy, efficiency, utility and useful operating life.
[0004] The standard method of cleaning a firearm includes the use of a patch of fabric cloth or a swab, attached to a cleaning rod. A large amount of copper buildup on the firearm typically requires some scraping with a sharp instrument to take off the bulk of the copper, prior to using the cleaning rod. The cloth or swab is then impregnated with cleaning solution, and the cleaning rod is run back and forth through the barrel (bore). Typical cleaning solutions include strong solvents and/or ammonia, which break down the various residues. The cloth or swab is frequently replaced so as not to transfer residues from one part of the firearm to another. A brass brush is typically connected to the cleaning rod and inserted vigorously through the barrel and the cylinders to loosen and clean the metal and/or carbon residue on the components of the firearm. After using the brush, clean cloths or swabs are subsequently run through the barrel and the cylinders to remove any remaining cleaning solution and/or residue in the firearm. A protective oil is typically applied to the firearm components after cleaning, as a rust preventative.
[0005] This multi-step cleaning method is time-consuming and messy, and thus there is a tendency among firearms users to perform this task somewhat less frequently than would be desirable. For example, in the case of a small firearm such as a rifle, even an hour spent on cleaning will frequently not leave the weapon completely free of carbon and/or metal residues, especially copper. The result is incomplete cleaning, resulting in deterioration in firearm performance. Similar problems exist for larger armaments, such as artillery.
[0006] Although typical cleaners satisfactorily remove some of the residues in firearms, they frequently suffer from certain disadvantages. For example, many cleaners are of low effectiveness in removing copper deposits. Some cleaners have a deleterious effect on the metal parts of the firearm (e.g. etching or embrittlement of the metal) which can adversely effect the accuracy of the firearm and/or cause the firearm to become unsafe or unreliable to use.
[0007] Many commonly used cleaners include highly volatile components which are flammable and/or have relatively low flash points, thus requiring special care during use. Many cleaners comprise solvents that are highly toxic and require special care, including the use of ventilated environments and the wearing of gloves and/or other handling equipment during firearm cleaning. Some cleaners include abrasives and/or require the addition of abrasives during the cleaning process, with the attendant possibility of scratching and/or damaging the firearm. Thus, commonly used cleaners can be inconvenient to use, store and/or handle, and can be very time-consuming to use.
[0008] There is a continued need for compositions and methods of cleaning gun bores employing means that are effective in removing copper and other deposits, without the need to resort to the use of flammable organic solvents or ammonia.
SUMMARY OF THE INVENTION
[0009] In one aspect, the invention is a composition for removing copper from a surface, the composition comprising between 0.5 wt. % and 15.0 wt. % of a polyphosphonic acid, between 1.0 wt. % and 40.0 wt. % of a hydroxyl-substituted primary amine, and water, and having a pH between 9.0 and 12.5.
[0010] In another aspect, the invention is a composition for removing copper from a surface, the composition comprising a polyphosphonic acid, a hydroxyl-substituted secondary amine, a surfactant, and water, and having a pH between 9.0 and 12.5
[0011] In yet another aspect, the invention is a composition for removing copper from a surface, the composition comprising a polyphosphonic acid, an amino acid, a surfactant, and water, and having a pH between 9.0 and 12.5.
[0012] In a further aspect, the invention is a composition for removing copper from a surface, the composition comprising a polyphosphonic acid, a compound comprising a nitrogen-containing heteroaromatic ring, a surfactant, and water, and having a pH between 9.0 and 12.5.
[0013] In a still further aspect, the invention is a method of removing copper from a surface, the method comprising contacting the surface with a composition comprising a polyphosphonic acid, a primary amine, and water to effect a removal of the copper.
[0014] In yet a further aspect, the invention is a method of cleaning a gun bore, the method comprising contacting the bore with a composition comprising a polyphosphonic acid, a primary amine, and water.
DETAILED DESCRIPTION OF THE INVENTION
[0015] The invention provides compositions and methods for removing copper from a surface. It will be understood that, as used herein, reference to removal of copper from a surface includes removal of brass from a surface. In one embodiment, the surface comprises a metal, with steel being one nonlimiting example. In one particular embodiment, the compositions of this invention are used to remove copper from the surface of high-grade steels, such as for example stainless steel 300 and 400 series, 4140 series and other chromium-molybdenum ordnance grade alloys. In another particular embodiment, the invention provides compositions and methods for removing copper deposits from gun bores, and/or cylinders, such as in a revolver. The compositions do this without using ammonia, which produces an irritating odor in compositions that employ it, and without the use of petroleum solvents.
[0016] Compositions according to the invention comprise a polyphosphonic acid, an amine, and water. The water is typically deionized. The compositions may also comprise other ingredients useful for removing other surface contaminants, for example carbon deposits and/or grease, from the treated surface. It will be understood that, once incorporated into the composition, the polyphosphonic acid and the amine may to a great extent be in the form of salts. This may be true for other ingredients as well. Thus, for simplicity, compositions recited herein are recited on the basis of the unreacted components as named, even though they may to some extent have changed form in the final composition.
Polyphosphonic Acid
[0017] The term “polyphosphonic acid”, as used herein, means a compound comprising two or more phosphonic acid moieties per molecule. A wide variety of polyphosphonic acids is suitable for use according to the invention. In one exemplary embodiment, the polyphosphonic acid comprises a polymethylenephosphonic acid according to formula I
[0000] (HO) 2 P(O)CH 2 —R 1 —CH 2 (O)P(OH) 2 I
[0000] wherein R 1 is a divalent organic radical which may comprise additional phosphonic acid groups. In one embodiment of the invention, R 1 may comprise a structure according to formula II
[0000] —NR 3 —R 2 —NR 4 - II
[0000] wherein R 2 is a divalent organic radical which may comprise additional phosphonic acid groups, and R 3 and R 4 are each separately hydrogen or an alkyl group having from one to twenty carbon atoms.
[0018] Suitable polyphosphonic acids for use according to the invention may include for example polymethylenephosphonic acids. One exemplary group of such materials comprises compounds with an ethylenediamine or polyethylenediamine backbone, and having a structure according to formula III
[0000] R 5 —(—NR 6 —CH 2 —CH 2 -) n —NR 7 R 8 III
[0000] wherein n is an integer from 1 to 10, and each of R 5 , R 6 , R 7 , and R 8 is independently hydrogen, a hydrocarbyl group having from one to twenty carbon atoms, and a phosphonomethyl group, provided that at least two of R 5 , R 6 , R 7 , and R 8 are phosphonomethyl groups. In one exemplary group of polyphosphonic acids according to the invention, n is from 2 to 5 and all of R 5 , R 6 , R 7 , and R 8 are phosphonomethyl groups. Examples of such compounds include ethylenediaminetetramethylenephosphonic acid and diethylenetriaminepentamethylenephosphonic acid (DTPMP). DTPMP is available from Solutia of St. Louis, Mo.
[0019] Other suitable examples of polyphosphonic acids for use according to the invention include polyethylenediamines wherein two or more nitrogen atoms in the backbone each bear at least one phosphonomethyl moiety substituted thereon, and/or wherein the polyphosphonic acid comprises at least one nitrogen atom bearing at least two phosphonomethyl moieties substituted thereon. Further suitable examples of polyphosphonic acids include 1-hydroxyethane-1,1-diphosphonic acid, aminotrimethylenephosphonic acid, hexamethylenediaminetetramethylenephosphonic acid, 2-hydroxyethyliminobis(methylenephosphonic acid), and bis(hexamethylene)triaminepentamethylenephosphonic acid. Although a number of exemplary polyphosphonic acids are recited above to illustrate the variety of polyphosphonic acids that may be suitable for use according to the invention, any polyphosphonic acid may be used. It will be understood that mixtures of polyphosphonic acids may also be used in accordance with the invention. The polyphosphonic acid, or mixture of acids, typically constitutes at least 0.5 wt. % of the composition, preferably at least 2.0 wt. %, and more preferably at least 3.5 wt. %. It typically constitutes at most 15.0 wt. % of the composition, preferably at most 8.0 wt. %, and more preferably at most 6.0 wt. %. However, amounts of polyphosphonic acid outside of these ranges may also be used.
Amine
[0020] Compositions according to the invention also comprise an amine, which may be a primary amine, a secondary amine, and/or a compound comprising a nitrogen-containing heteroaromatic ring such as a substituted or unsubstituted pyridine, pyrimidine, triazine, pyrrole, bipyridine, ring-substituted derivative of these, and/or ring-fused derivative of these, such as for example substituted or unsubstituted benzimidazole and substituted or unsubstituted benzoxazole.
[0021] Typically the amine comprises a primary amine. In one exemplary embodiment of the invention, suitable primary amines may include alkylamines wherein the alkyl substituent comprises from five to twenty carbon atoms. In another exemplary embodiment, the primary amine comprises a hydroxyl-substituted primary amine, including as nonlimiting examples vicinal alkanolamines such as ethanolamine and isopropanolamine. Other suitable primary amines may include polyamines. One exemplary group of suitable polyamines includes ethylenediamine and polyethylenediamines, such as for example diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenexhexamine, and higher homologs. Terminal diamines such as hexamethylenediamine and tetramethylenediamine may also be used, as may homologs of diethylenetriamine such as bis(hexamethylene)triamine.
[0022] Amino acids may also be used according to the invention, to provide the amine. In certain cases, for example where the amine is an amino acid or a hydroxyl-substituted amine or a polyethylene diamine, the composition may have a very low odor. Although a number of exemplary amines are recited above to illustrate the variety of amines that may be suitable for use according to the invention, any amine may be used. It will also be noted that mixtures of amines may also be used in accordance with the invention, and may comprise any combination of primary, secondary, and tertiary amines. Further, it will be understood that amines suitable for use according to the invention may comprise a combination of primary, secondary, and/or tertiary amine functionality in a single molecule.
[0023] In one embodiment of the invention, the composition may comprise a dialkanolamine and/or a trialkanolamine, either alone or in combination with another amine, for example a primary amine. If a combination of primary amine with a dialkanolamine and/or a trialkanolamine is used, the primary, secondary, and/or tertiary amine groups may or may not be in the same molecule. In one particular embodiment, the other amine comprises an alkanolamine such as ethanolamine. Nonlimiting examples of suitable dialkanolamines and trialkanolamines include diethanolamine, diisopropanolamine, and triethanolamine. The use of such a component may, inter alia, allow for more facile adjustment of the pH of the composition, which may be beneficial to its activity in removing copper and/or other residues from the surface being treated.
[0024] Without wishing to be bound by any particular theory or explanation, it is believed that the amine complexes copper species, facilitating removal of copper from the surface being treated. The amine, or mixture of amines, typically constitutes at least 1 wt. % of the composition, preferably at least 10 wt. %, and more preferably at least 18 wt. %. It typically constitutes at most 40 wt. % of the composition, preferably at most 30 wt. %, and more preferably at most 20 wt. %. However, amounts outside of these ranges may also be used.
[0025] In the case where the amine comprises a mixture of amines, of which a dialkanolamine and/or trialkanolamine is a portion, the dialkanolamine(s) and/or trialkanolamine(s) may together constitute at least 0.5 wt. % of the total amine in the composition, preferably at least 1.0 wt. %, and more preferably at least 2.8 wt. %. They may constitute at most 9.0 wt. % of the amine in the composition, preferably at most 6.0 wt. %, and more preferably at most 3.2 wt. %. One exemplary embodiment of a composition comprising a combination of amines is as follows, with the amounts given on a parts by weight basis.
[0000]
Deionized Water
55.00
Monoethanolamine
18.00
Triethanolamine
0.28
Propylene Glycol
18.50
Diethylenetriaminepentamethylenephosphonic acid
3.22
Ethoxylated propylated fatty alcohol
4.00
Amine carboxylate
1.00
Degreaser
[0026] Compositions according to the invention may optionally comprise a degreaser, which may for example be useful in formulations for cleaning gun barrels (bores) that have lubricants and and/or other oily or hydrophobic contaminants in them. Nonlimiting examples of degreasers suitable for use according to the invention are ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, and glycol dialkyl ethers derived from mono- or di-ethylene glycol or from mono- or di-propylene glycol. Other suitable degreasers include polyglycols, for example polyethylene glycols and polypropylene glycols. Methyl glycine may also be used. In one exemplary embodiment, the degreaser comprises propylene glycol alone.
[0027] It will be understood that mixtures of degreasers may also be used in accordance with the invention. The degreaser, or mixture of degreasers, may constitute at least 1 wt. % of the composition, preferably at least 10 wt. %, and more preferably at least 18 wt. %. It may constitute at most 65 wt. % of the composition, preferably at most 40 wt. %, and more preferably at most 19 wt. %.
Surfactant
[0028] Compositions according to the invention may optionally comprise a surfactant, which may for example be useful in formulations for cleaning gun barrels (bores) that have carbon deposits or other contaminants in them. Suitable surfactants may be cationic, anionic, nonionic, or a combination of any of these. Many suitable surfactants are known in the art and are widely available commercially. Nonlimiting examples of surfactants suitable for use according to the invention include the following.
[0029] Exemplary anionic surfactants suitable for use according to the invention include carboxylates such as alkylcarboxylates (carboxylic acid salts) and polyalkoxycarboxylates, alcohol ethoxylate carboxylates, nonylphenol ethoxylate carboxylates, and the like; sulfonates such as alkylsulfonates, alkylbenzenesulfonates, alkylarylsulfonates, sulfonated fatty acid esters, and the like; sulfates such as sulfated alcohols, sulfated alcohol ethoxylates, sulfated alkylphenols, alkylsulfates, sulfosuccinates, alkylether sulfates, and the like; and phosphate esters such as alkylphosphate esters, and the like. Preferred anionics are sodium alkylarylsulfonate, alpha-olefinsulfonate, salts of linear alkyl benzenesulfonates, sodium lauryl ether sulfate, and fatty alcohol sulfates.
[0030] Suitable exemplary cationic surfactants include quaternary ammonium salts, for example alkylquaternary ammonium chloride surfactants such as n-alkyl (C 12 -C 18 ) dimethylbenzylammonium chloride, n-tetradecyldimethylbenzylammonium chloride monohydrate, a naphthalene-substituted quaternary ammonium chloride such as dimethyl-1-naphthylmethylammonium chloride, and the like.
[0031] Exemplary nonionic surfactants suitable for use according to the invention include those having a polyalkylene oxide polymer as a portion of the surfactant molecule. Such nonionic surfactants include, for example, benzyl-, methyl-, ethyl-, propyl-, butyl- and other like alkyl-capped polyethylene glycol ethers of fatty alcohols; polyalkylene oxide free nonionics such as alkyl polyglycosides; sorbitan and sucrose esters and their ethoxylates; alkoxylated ethylene diamine; alcohol alkoxylates such as alcohol ethoxylate propoxylates, alcohol propoxylates, alcohol propoxylate ethoxylate propoxylates, alcohol ethoxylate butoxylates, and the like; alkylphenol ethoxylate, polyoxyethylene glycol ethers and the like; carboxylic acid esters such as glycerol esters, polyoxyethylene esters, ethoxylated and glycol esters of fatty acids, and the like; carboxylic amides such as diethanolamine condensates, monoalkanolamine condensates, polyoxyethylene fatty acid amides, and the like; ethoxylated alcohols, ethoxylated amines, and polyalkylene oxide block copolymers including an ethylene oxide/propylene oxide block copolymers. Silicone surfactants may also be used. One particular nonionic surfactant suitable for use is Rhodaclean™ ASP (ethoxylated propylated fatty alcohol), available from Ashland Distribution Company of Covington, Ky. or from Rhodia Inc., Cranbury, N.J.
[0032] It will be understood that mixtures of surfactants may also be used in accordance with the invention. The surfactant, or mixture of surfactants, may constitute at least 0.1 wt. % of the composition, preferably at least 1.0 wt. %, and more preferably at least 3.7 wt. %. It may constitute at most 15.0 wt. % of the composition, preferably at most 7.0 wt. %, and more preferably at most 4.3 wt. %.
Other Ingredients
[0033] The composition may comprise other ingredients for improving various performance aspects in certain use applications. For example, the composition may contain a rust inhibitor, if the surface to be treated comprises iron or steel. An exemplary rust inhibitor is an amine carboxylate sold under the name Thorcor CI-20 by Thornley Company Incorporated, Wilmington, Del. Still other ingredients may be added to suit particular application needs.
[0034] In one exemplary embodiment, compositions according to the invention may comprise a combination of ingredients falling within the ranges shown in the following table, where “lower” and “upper” refer to weight percent in the total formulation.
[0000]
INGREDIENT
Lower
Upper
Water
5.0
85.0
Diethylenetriaminepentamethylenephosphonic acid
0.5
15.0
Ethanolamine
1.0
25.0
Propylene Glycol
1.0
65.0
Ethoxylated Propylated Fatty Alcohol
0.1
15.0
Amine Carboxylate
0.1
5.0
[0035] Compositions according to the invention may in general be prepared by mixing the ingredients in any sequence.
[0036] Compositions according to the invention have a pH of at least 9.0, preferably at least 11.0, and at most 12.5, preferably at most 11.5. It will be appreciated that a wide variety of combinations of the ingredients outlined above is possible according to the invention, and that adjustment of pH to the desired range may or may not be needed in order to fall within acceptable limits, depending upon the exact formulation used. If necessary, pH may be adjusted upward by addition of monoethanolamine, and may be adjusted downward by the addition of diethylenetriaminepentamethylenephosphonic acid.
[0037] Use of the compositions of this invention to remove copper from a surface is typically performed by contacting the surface to be cleaned with the composition at ambient temperature, although higher or lower temperatures may be used. The contacting may be by any of a variety of means, for example by application with a brush, roller, sprayer, or impregnated cloth or the like, or by dipping the article to be treated into the composition. The composition is typically allowed to contact the surface for a period of time, that period being dependent on the exact surface being treated, the temperature, the nature and amount of copper and other residues or contaminants on the surface, and other variables. Most commonly, the composition is then removed from the surface, although this need not always be done. If it is removed, it may be done by any commonly practiced means such as rinsing, wiping with a cloth, or the like.
[0038] In the case where the surface being treated is that of a gun bore, a contact time between 30 seconds and 5 minutes is typical, particularly if the composition comprises a primary amine. For cleaning a gun bore, standard methods of application of the composition are suitable. This may typically comprise using a patch of fabric cloth or a swab, impregnated with the composition and attached to a cleaning rod. The cleaning rod is run back and forth through the barrel (bore). A brass brush may also be used, but is typically not needed. After using composition and optionally the brush, clean cloths or swabs are typically run through the barrel and the cylinders to remove any remaining cleaning solution and/or residue in the firearm. A protective oil is typically applied to the firearm components after cleaning, as a rust preventative, but this is optional.
EXAMPLES
[0039] The effects of using a combination of a primary amine and polyphosphonic acid were investigated by mass loss experiments on copper metal coupons. Three formulations were tested at room temperature by immersing weighed copper panels in each formulation for four minutes, rinsing with deionized water, drying in an oven for 15 minutes, allowing to cool to room temperature, and reweighing to determine the mass lost. An etch rate for each formulation was then calculated based on the 0.052 square foot area of each coupon. The formulation amounts are given in wt. %. The ethoxylated propylated fatty alcohol was Rhodaclean™ ASP, and the amine carboxylate was Thorcor CI-20.
[0000]
INGREDIENT
1
2
3
Water
58.5
73.0
55.0
Diethylenetriaminepenta-
3.22
3.22
methylenephosphonic acid
Ethanolamine
18.0
18.0
Triethanolamine
0.28
0.28
Propylene Glycol
18.5
18.5
18.5
Ethoxylated Propylated Fatty Alcohol
4.0
4.0
4.0
Amine Carboxylate
1.0
1.0
Coupon Mass (grams, before etch)
9.4283
10.0931
10.2815
Coupon Mass (grams, after etch)
9.4282
10.0925
10.2782
Copper Mass Lost (grams)
0.0001
0.0006
0.0033
Copper Etch Rate (mg/ft 2 /min)
0.48
2.87
15.75
[0040] The data indicate that the combination of a primary amine with DTPMP offers a vastly increased etch rate on copper metal compared with either constituent alone. This property is of great importance when used to clean ordnance of copper or brass residues in a timely manner.
[0041] Although the invention is illustrated and described herein with reference to specific embodiments, the invention is not intended to be limited to the details shown. Rather, various modifications may be made in the details within the scope and range of equivalents of the claims and without departing from the invention. | A method of removing metallic copper from a steel surface defining a bore or cylinder of a gun is provided. The method involves contacting the surface with a composition comprising a polyphosphonic acid, a hydroxyl-substituted primary amine, and water. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
The present patent application is a divisional application of commonly assigned U.S. patent application Ser. No. 13/746,042, itself claiming priority of U.S. Provisional Patent Application No. 61/736,270, entitled “Prefabricated Energy Efficient Data Center Condominiums and Method of Large Scale Deployment” and filed at the United States Patent and Trademark Office on Dec. 12, 2012. The present application claims the benefits of priority of all these prior applications. The disclosures of these prior applications are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention generally relates to data centers and more particularly to modular data centers and data center modules.
BACKGROUND OF THE INVENTION
Modularity, scalability and flexibility are now essential requirements for efficient and cost effective data centers. Modularity is the building block that allows rapid on-demand deployment of infrastructures. Modularity minimizes capital expenditure and, thus, maximizes return on investment (ROI). Scalability relates to modularity, but is the additional key that enables a design to scale past the barrier of a predetermined fixed number of modules. It is the glue that allows the different types of modules to coherently scale: specifically computing modules with floor/space modules, power modules, and cooling modules. Flexibility further refines modularity and scalability by allowing any type of hardware from any vendor, with various power and cooling requirements, to coexist within the same data center. It is most crucial in the context of serving multiple independent users choosing to collocate their specific computing machinery in a shared data center.
Recent power density increases in computer packaging are amongst the greatest limiting factors of scalability and flexibility in data centers. Current best practices suggest to partition large computing rooms into low, medium, and high power density zones. In this way, a limited form of scalability and flexibility can be reached, negating the need to overprovision the whole computing room with the highest possible power density capability. Nevertheless, forcing these zones to be sized a priori is hardly modular. The problem lies with the conventional data center design where a huge computing room is surrounded by proportionally sized mechanical and electrical rooms. Such arrangements are difficult to scale, because large distances limit our ability to efficiently distribute low voltage power to computing machinery, and move enough air to keep this machinery cool. Air cooling at large scales especially becomes daunting, because air velocity needs to be kept at acceptable levels using air conduits with limited cross-sections. Too much air velocity brings turbulence that in turn produces pressure differentials and, thus, non uniform air distribution and poor cooling efficiency. Moving water over large distances is both much easier and efficient. However, bringing water all the way to the computer cabinet (or even inside the cabinets) creates other challenges like leak detection and proofing.
Another popular trend is to use shipping containers to host preconfigured and preassembled computing hardware. Although this approach can be very modular and, to some extent, scalable, it is not so much flexible. The physical dimensions of a standard shipping container impose severe space constraints that usually limit the computer form factors that can be hosted while rendering hardware maintenance operations more difficult. Promoters of this approach are often hardware vendors of some sort, using the container model to push their own hardware as the backbone of data centers. Container based data centers are most practical when computing resources need to be mobile for some reason. In practice, however, even though rapid initial deployment is an obvious competitive advantage, rapid redeployment is a rare requirement because of the relative short lifespan of computers. Moreover, there is the additional issue of the low voltage power feeds usually required by these containers that have limited space for in-container power transformation. For large scale configurations, this forces either to inefficiently carry low voltage energy over large distances, or to combine computing containers with power transformation containers.
Finally, energy efficiency is also a very important requirement for modern data centers, both because of its financial and environmental impact. The two main sources of power losses in data centers lie in voltage transformation and regularization, on the one hand, and heat disposal, on the second hand. Best practices for efficient electrical systems are to minimize the number of voltage transformation stages and to transport energy at higher voltage. Also, it is important to correctly size the electrical infrastructure according to effective needs, as underutilized electrical systems are usually less efficient. As for efficient heat disposal, there are mostly air-side and water-side economizers to exploit favorable outside climate conditions to totally or partially circumvent the need for power hungry chillers. The holistic problem, however, is how to design cost-effective and energy efficient data centers that are also modular, scalable, and flexible.
In view of the foregoing, there is a need for an improved data center module which mitigates at least some shortcomings of prior data center modules.
SUMMARY OF THE INVENTION
A data center module in accordance with the principles of the present invention generally mitigates at least some of the shortcomings of prior data center modules by comprising multiple levels configured to accommodate both the cooling and the electric subsystems and the computing machinery (e.g. servers), and by being configured to be deployed with other identical data center modules around a central shared facility.
A data center module in accordance with the principles of the present invention generally comprises a compact-footprint weatherproof envelop, complete with party walls and staging areas, and a multistory energy efficient layout capable of powering and cooling typically generic computer hardware. The module therefore generally comprises all necessary voltage power transformation, power regularization (e.g. UPS), power distribution, and cooling subsystems. This configuration generally allows the simultaneous optimization of the power capacity density and hosting flexibility at very large scales.
A data center module in accordance with the principles of the present invention generally comprises an outer envelop and a plurality of levels, the plurality of levels being superimposed one over the other and comprising a bottom level and at least two upper levels, the at least two upper levels comprising a plurality of computing machines, the plurality of levels being in fluid communication thereby allowing downward and upward movements of air within the module. The module comprises an air handling unit, the air handling unit being in fluid communication with the top of the at least two upper levels, wherein each of the plurality of levels is partitioned into a first area and a second area; the first areas of the plurality of levels are in fluid communication to allow downward movements of air within the module, and wherein the second areas of the plurality of levels are in fluid communication to allow upward movements of air within the module; the first area and the second area of the bottom level are in fluid communication to allow air moving downwardly into the first area to transfer upwardly into the second area; the computing machines are located in one of said first area or said second area of each of the at least two upper levels; the computing machines are arranged in at least one row, and wherein the at least one row defines at least two aisles; the at least two aisles comprise at least one cold aisle located on one side of the at least one row of computing machines, the at least one cold aisle carrying cooling air toward the computing machines, and wherein the at least two aisles comprise at least one hot aisle located on the other side of the at least one row of computing machines, the hot aisle carrying warmed cooling air flowing out of the computing machines; the at least one hot aisles have non decreasing cross-section when flowing from one level to the next.
In typical yet non-limitative embodiments, the data center module is configured to be prefabricated and be deployed in clusters of other identical (at least externally) data center modules juxtaposed both side-by-side and back-to-back without interleaving between adjacent modules.
In typical yet non-limitative embodiments, the data center module has a 30-feet by 40-feet footprint, e.g. the equivalent of three 40-feet long shipping containers laid out side-by-side. It can accommodate different power density and cooling requirements in various redundancy configurations. It combines the advantages of the conventional “brick-and-mortar” data center with those of the container based data center, without their respective limitations. Typically using mostly standardized off-the-shelf electrical and mechanical components, it is modular and prefabricated to allow fast on-demand deployments, adding capacity in sync with user needs. It can efficiently host most any type of computing equipment with any type of power density requirement. For instance, power densities of over 30 kilowatts per cabinet are possible using air-cooled computer hardware. Cabinets that require chilled-water feeds, for instance to support rear-door heat exchangers, are also possible, even though rarely required if designed for front-to-back air circulation. Moreover, low density cabinets can coexist side-by-side with high density ones, without creating cooling problems. For maintenance, large aisles are provided for unconstrained access to both the front and rear of compute cabinets.
Typically, a module has a ground floor for hosting its power and cooling subsystems, and several upper floors for hosting its computer cabinets. It is designed to be self-contained and weatherproof. Its maximum power envelope is determined by the capacity of its user specified electrical infrastructure (up to 1.2 megawatts for a typical 30-feet wide unit). Given this infrastructure, the number of upper floors can be adjusted to match the power density requirements: less floors for higher density; more floors for lower density. The data center modules are designed to accommodate any size of air-cooled computer cabinets, as long as air circulation is front-to-back. The maximum allowable number of cabinets is a function of the cabinet width and of the number of upper floors. For instance, a 30-feet wide by 40-feet deep unit provides up to two 32-feet rows of linear space that can accommodate up to 32 standard size (24-inch wide; 15 per row) cabinets per floor. The average allowable power dissipation per cabinet is simply determined by dividing the total power envelope of the module with its total number of cabinets. For instance, a module with a 1.2 megawatts power envelop and three computing floors can host up to 96 cabinets, each dissipating 12.5 kilowatts on average.
With four floors, 128 cabinets could be accommodated with an average power consumption of 9.4 kilowatts. The cooling system allows for any mixture of low, medium or high power density cabinets, as long as the total power consumption is below the power envelope of the module.
Herein, low power density typically refers to 5 kilowatts or less per cabinet, medium density typically refers to between 5 and 15 kilowatts per cabinet, and high density typically refers to more than 15 kilowatts per cabinet. However, such ranges are likely to change over time.
In accordance with the principles of the present invention, though each data center module is mostly autonomous, it is configured to be deployed around a central facility responsible for providing reliable low or medium voltage power feeds that can efficiently be carried over distances of several hundreds of feet to modules, in a cost-effective and energy efficient way.
Herein, low voltage is typically defined as below 1 kilovolt, while medium voltage is typically between 1 and 30 kilovolts. The central facility typically includes the usual medium voltage power generators and transfer switch-gears that provide backup energy in case of grid failure. It can also include any high-to-medium voltage transformation gear that is necessary if the utility company energizes the central facility with a high voltage power line. Herein, high voltage typically refers to above 30 kilovolts.
The central facility typically further includes high efficiency modular chilled-water production subsystems, optimized for the local climate using water towers or any other water-side economizer mechanisms. The rational for centralizing the chilled-water service revolves around the following three motivations. First, on a yearly basis, it is expected that most of the cooling necessary for a module can be realized using an air-side economizer cycle based on outside fresh air. Thus, there is no need for providing necessarily undersubscribed and inefficient local chilled-water production capacity. The air-side economizer cycle is built into the prefabricated module because, contrary to water, air cannot efficiently be distributed over large distances; it needs to be handled locally. Second, large industrial chillers can be made very efficient, much more than any other direct exchange (DX) cooling system small enough to fit inside a module. If all cooling cannot be realized using an air-side economizer cycle, centralizing the chilled-water production is still an effective way of minimizing the power usage efficiency (PUE) of the data center. Third, if it is practical to reuse the heat generated by the computing machinery for other means, for instance to heat adjacent buildings during winter, then the chilled-water loop must also be centralized to maximize the energy reuse effectiveness (ERE) of the data center complex.
Thus, whenever practical, to enable energy reuse, the central facility can signal the modules that they should use as much chilled-water as necessary, by recycling the wasted hot air in a closed-loop, transferring the corresponding energy into the water return of the chilled-water loop. Otherwise, if no more energy reuse is possible, the modules will try to minimize the PUE by using as little chilled-water as possible, instead favoring free air cooling, breathing outside fresh air, circulating this air through computer cabinets and exhausting the wasted hot air to the outside.
Finally, the central facility is also responsible for providing other shared services, for instance points of presence for Internet providers, security check points and biometric access controls, loading docks, meeting rooms, etc.
In typical yet non-limitative embodiments, the central facility is connected to scalable clusters of data center modules using segregated passage ways for power feeds, chilled-water loops, communication network cables (e.g. fiber-optic cables), and human access. Data center modules are typically juxtaposed on both sides of a multistory corridor structure. The ground level corridor generally provides human access to the power and cooling subsystems, while the upper floor corridors are for accessing the computing levels. The chilled-water loop is typically placed underground, below the first corridor, while the power feeds are routed in the false ceiling of the same corridor. All communication network cables are typically routed in the false ceiling of the second level corridor.
In typical yet non-limitative embodiments, the data center module comprises an efficient cooling system combining in a single hybrid system the efficiency of both air-side and water-side economizers, without multiplying the number of system components. The air-side mode of operation, where the heat dissipated by the computing machinery is rejected into the atmosphere, is preferred when there is no practical way to reuse this heat, while the water-side mode of operation is used if the heat can be reused, for example to heat other nearby buildings. The system can efficiently operate partially in both modes (hybrid mode) when only part of the generated heat can be reused in a practical way.
The particular vertical, i.e. multistory, configuration of the data center module allows for cost-effective usage of a small number of large mechanical components that both increase efficiency and reliability, contrary to previous modular systems that rely on many more smaller components because of either cramped space constraints, or because forced-air circulation over long distances is too inefficient.
Other and further aspects and advantages of the present invention will be obvious upon an understanding of the illustrative embodiments about to be described or will be indicated in the appended claims, and various advantages not referred to herein will occur to one skilled in the art upon employment of the invention in practice. The features of the present invention which are believed to be novel are set forth with particularity in the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
The above and other aspects, features and advantages of the invention will become more readily apparent from the following description, reference being made to the accompanying drawings in which:
FIG. 1 a presents a perspective view of an embodiment of a large scale data center complex with a central facility building and 2 clusters of 32 prefabricated data center modules each, connected by a grid of corridors, in accordance with the principles of the present invention.
FIG. 1 b presents a perspective view of an embodiment of a central facility building with three data center modules, but with a corridor section and concrete slab ready for appending 5 additional prefabricated data center modules.
FIG. 2 a is a perspective view of an embodiment of a four-story prefabricated data center module shown with a weatherproof prefabricated weight bearing exterior shell or envelop in accordance with the principles of the present invention, the module comprising a ground floor for power and cooling subsystems, and three upper floors for computing machinery.
FIG. 2 b is a perspective view of an embodiment of a four-story prefabricated data center module shown without a weatherproof prefabricated weight bearing exterior shell or envelop in accordance with the principles of the present invention, the module comprising a ground floor for power and cooling subsystems, and three upper floors for computing machinery.
FIG. 3 is a plan view projection of the first upper floor of the prefabricated data center module of FIG. 2 , where computing equipments (e.g. servers) are located.
FIG. 4 is a plan view projection of the ground floor of the prefabricated data center module of FIG. 2 , where the power and cooling subsystems are located.
FIG. 5 is an elevation side view of the prefabricated data center module of FIG. 2 that shows part of the cooling subsystem on the ground floor and the arrangement of computer cabinets on the upper floors.
FIG. 6 is an elevation front view projection of the prefabricated data center module of FIG. 2 , illustrating its different internal airflow patterns.
FIG. 7 is a flowchart that illustrates an exemplary method for deploying large scale data center module complexes in accordance with the principles of the present invention.
FIGS. 8 a and 8 b is a flowchart that illustrates an exemplary all-season hybrid-loop control method for the cooling system of the prefabricated data center module in accordance with the principles of the present invention.
FIG. 9 is a flowchart that illustrates an exemplary closed-loop control method for the cooling system of the prefabricated data center module, in accordance with the principles of the present invention, when the outside air conditions do not permit the efficient use of an air-side economizer cycle.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Novel prefabricated data center modules and a method of their large-scale deployment will be described hereinafter. Although the invention is described in terms of specific illustrative embodiments, it is to be understood that the embodiments described herein are by way of example only and that the scope of the invention is not intended to be limited thereby.
Referring to FIG. 1 a , a module-based data center complex is shown at 10 to be composed of a main facility building 100 surrounded by clusters 205 of prefabricated data center modules or units 200 . In this case, 2 clusters 205 of 32 modules 200 each. The central facility 100 hosts the services that are shared by the modules 200 : low or medium voltage power feeds, chilled-water feeds, demineralized water for humidity control, Internet connections, security check points with biometric access controls, washrooms, meeting rooms, etc.
The data center modules 200 are linked to the central facility 100 by a grid of corridors 300 that not only insure secure human access, but also serve as passageways to distribute shared services.
The topology of module clusters 205 is not limited to the example shown in FIG. 1 a . In general, clustered modules 200 are juxtaposed on each side of a main corridor 310 , with possible orthogonal secondary corridors 320 , to both minimize the total footprint of clusters 205 and the distances over which services must be carried. However, any other topology can be used to accommodate different shapes of land. To maximize flexibility, the data center modules 200 are designed to be juxtaposed side-to-side and back-to-back without wasting any real estate as shown in FIG. 1 a.
The data center modules 200 are multistory to maximize density and decrease distances. The ground floor is used for mechanical and electrical subsystems, while the upper floors host the computing machinery (e.g. servers). The modules 200 are mostly autonomous; they only require a power feed and a chilled-water feed provided by the central facility 100 . They have their own voltage transformers, UPS(s), power distribution, and cooling system. All controls are embedded within each module 200 , but can be monitored and operated from the central facility building 100 , or remotely through secure network access.
The corridors 310 and 320 that link the main building 100 to the data center modules 200 are also multistory. The ground level corridors 312 and 322 provide human access to the ground level of the modules 200 while the upper floor corridors 314 and 324 are for accessing the upper computing levels (see FIG. 1 b ). All water feeds are typically carried under the ground level corridors 312 and 322 , and all power feeds are typically carried in the false ceiling of the same corridors. In this way, the effect of a water pipe fracture is minimized. All communication network feeds are routed in the false ceiling of the above ground corridors 314 and 324 .
In FIG. 1 b , three existing modules 200 are shown connected to the central facility building 100 by a corridor section 310 that can accept 5 additional modules; 1 on the same side of the corridor 310 as the first three modules 200 , and 4 on the opposite side. It should be noted that this corridor 310 is drawn with its walls removed for illustration purposes. In reality, it would be closed on both sides with reusable party walls.
This figure also illustrates the fact that a module-based data center complex 10 can be assembled on-demand, one module 200 at a time, after having built a corridor section 310 . Not shown are the emergency exits that are typically located at the end of corridors 310 and 320 .
Referring to FIG. 2 a and FIG. 2 b , each prefabricated data center module 200 comprises a ground level 210 for power and cooling subsystems, and several stories 230 for computing machinery. In this particular case, three computing stories 230 are shown. Each floor has an access door in the front, one door 212 on the ground floor, and one door 232 on each of the upper floors 230 . The ground level door 212 gives access to the module 200 power and cooling subsystems, while the upper level doors 232 provide access to the computing machinery. They open into the corridor passageways 312 and 314 of FIG. 1 b.
A module 200 has a weatherproof prefabricated weight bearing exterior shell or envelop 250 designed to be shared by adjacent modules 200 . In other words, in the present embodiment, a module 200 built adjacent to an existing module 200 will share a wall with the existing module 200 , thereby reducing costs and wasted spaces. Still, in other embodiments, each module 200 could have its own exterior envelop 250 without sharing adjacent wall(s).
The corridors 310 and 320 also share this modular structure so that a large scale data center complex 10 can be rapidly and efficiently assembled one module 200 at a time.
Still referring to FIG. 2 a and FIG. 2 b , an air handling unit 270 is located on the rooftop 260 of the module 200 to allow an optimized cooling system that can benefit from both air-side or water-side economizers, while effectively minimizing its real-estate footprint. When climate is favorable, the cooling system draws outside air through one or more intake vents 272 and moves this cold air downward to the ground floor 210 . The cold air is then pushed upwards to cool the computers located on the upper floors 230 , and the generated hot air is either exhausted through one or more exhaust vents 274 located at the top part of the air handling unit 270 , or recirculated by mixing it with the intake air. The air handling unit 270 is designed in such a way that exhausted air cannot recirculate through the intake vents 272 . In that sense, the exhaust vents 274 of the air handling unit 270 are located higher than the intake vents 272 as best shown in FIG. 2 b . Moreover, the air intake is recessed from the module's side so that adjacent modules 200 can be attached side-by-side without wasting any interleaving space at the ground level, and without any mutual interference. Both intake and exhaust vents 272 and 274 are respectively equipped with motorized dampers 276 and 278 (see FIG. 6 ) that can control their effective cross-sections and, thus, the volume of air per unit of time that can enter and exit the module 200 . When climate is unfavorable, or if there is a possibility of heat reuse, these dampers 276 and 278 are fully closed and the cooling system uses the chilled-water loop provided by the central facility 100 to cool the closed-loop recirculated air.
FIG. 3 gives a plan view projection of the first upper floor 230 of the module 200 . Each upper floor 230 is divided into three rooms or areas by a drywall 231 . The first room is a general purpose staging area 234 that communicates with the external access corridor through the entrance door 232 . The second is an air handling area 236 that links the rooftop air intake 272 to the ground floor 210 . The air handling area 236 typically comprises one or more fans 237 for pushing the air from the air handling unit 270 toward the ground floor 210 . The third is a computing room 238 that comprises, in the present embodiment, two cold-aisles 239 separated from a central hot-aisle 241 by two parallel rows of computer cabinets 240 . Understandably, in other embodiments, the number of cold-aisle(s), hot-aisle(s) and row(s) of computer cabinets could be different. For example, in some embodiments, there could be one cold aisle, one hot aisle, and one row of computer cabinets, and in still other embodiments, there could be three cold-aisles, two hot-aisles and four rows of cabinets.
Three doors 246 provide access from the staging area 234 to the three aisles 239 and 241 of the computing room 238 , and a fourth door 248 is for accessing the air handling area 236 .
Through grating in the floor (see also FIG. 6 ), the cold-aisles 239 are connected from the ground floor 210 to the top floor 230 , creating a vertical plenum of cold air. The central hot-aisle 241 is connected from the first floor 230 to the rooftop air handling unit 270 , forming another vertical plenum. By traversing the compute cabinets 240 , from cold-aisle 239 to hot-aisle 241 , the computing machinery can effectively be cooled by transferring the generated heat to the airflow.
For a typical 30-feet wide by 40-feet deep module 200 , there is room for 32 linear feet of cabinets 240 per row, which is enough to host up to 32 standardized 24-inch wide cabinets 240 per floor. The last cabinet 242 at the end of each row 240 , the one nearest to the drywall 231 , can be used to accommodate any necessary voltage transformers. Power is typically distributed to the compute cabinets using overhead busbars 244 .
Wider modules 200 can accommodate more cabinet aisles 240 using the same principle. Similarly, deeper modules 200 can accommodate longer aisles with more cabinets 240 per row.
The maximal power envelop of a module 200 is determined by two main limiting factors: the capacity of its power and cooling subsystems (transformers, UPSs, fans, and coils) and the width of the grating section of its cold-aisles 239 on the first floor 230 , which determines the maximum velocity of the upward air flow. This is a limiting factor, because too much velocity creates turbulence which in turn induces differences in pressure and temperature. It typically needs to be kept under 5 meters per second (1000-feet per minute) so that the cold-aisle 239 can behave as a plenum and, thus, eliminate all possibilities of non-uniform cooling. For the typical module 200 of FIG. 3 with its 4-feet and a half wide cold-aisles 239 , assuming that compute servers can effectively be cooled using an airflow of 100 CFM per kilowatt of heat dissipation, at 20-degree Celsius, this translates to a possible power envelop of up to 2.4 megawatts for 96 cabinets, or 25 kilowatts per cabinet on average. For a more typical configuration with cabinets dissipating on average 12 kilowatts, the maximum air velocity drops well below the critical threshold.
As for air velocity in the central hot-aisle 241 , it is much less critical, because turbulence there will not affect the cooling of the computing machinery.
Notably, this configuration enables the electrical subsystems of the module 200 to be air-cooled with the same system used for cooling the computing machinery. No addition components are necessary.
Referring to FIG. 4 , the ground floor 210 of the module 200 is also divided into three rooms or areas: an entrance hall 214 that can host fire protection systems, for instance, an electrical room 216 that can host heat producing electrical components like transformers and UPSs, and a positive pressure intake plenum area 218 . The airflow is forced downward from the above air handling area 236 (see FIGS. 3 and 6 ) using a set of variable drive fans 237 . It then traverses to the electrical room 216 through filters 220 and cooling coils 222 before moving upward through the grating floor of the above cold-aisles 239 , carrying any heat dissipated by the electrical components located in the electrical room 216 .
Referring to FIG. 5 , the module 200 is divided logically into three vertical parts: a lower part 292 for the electrical and mechanical components, including cooling coils 222 , a multilevel middle part 294 for the computing machinery 240 , and an upper part 296 for the air handling unit 270 with its intake vents 272 and exhaust vents 274 .
FIG. 6 provides a detailed elevation view of the various airflows inside the present embodiment of the data center module 200 . It indicates the three vertical parts of the module: lower part 292 , middle part 294 and upper part 296 ; and illustrates that each part can be further subdivided into a left-hand side 293 , and a right-hand side 295 . It shows the different system components: filter banks 220 , cooling coil sets 222 , variable drive fans 237 , humidifiers 224 , intake vent 272 with dampers 276 , exhaust vent 274 with dampers 278 , computing cabinets 240 , upward vertical hot-aisle 241 , upward vertical cold-aisles 239 , air mixing dampers 275 , downward mixing plenum 236 , input plenum 218 , cold plenum 216 , exhaust plenum 277 , and optional UPS submodule(s) 217 .
Starting from the input plenum 218 that is under a positive pressure created by the fans 237 , the air first crosses the filters banks 220 and coils 222 . Depending on the mode of operation, this input air can be either hot or cold. In closed-loop operations, being recirculated from the hot-aisle 241 through the exhaust plenum 277 , mixing dampers 275 , and mixing plenum 236 , the air is warm and may need to be cooled by the coils 222 . In hybrid-loop operations, coming mostly from the outside through the intake vent 272 , it may be cold enough to not require any cooling, but it may also be too cold. In that case, it is heated using the warm air from the exhaust plenum 277 , by mixing part of it through the mixing dampers 275 . Then, whatever warm air from the exhaust plenum 277 not used for mixing will naturally exit through the exhaust vents 274 .
Once the air crosses to the central cold plenum 216 , it can rise through the grating floors of the cold-aisles 239 and reach the servers in the computer cabinets 240 . From there, through the computer cabinets 240 , it crosses to the hot-aisle 241 , absorbing the heat dissipated by the servers. The rows of cabinets 240 need to form a sealed barrier between the cold-aisles 239 and hot-aisle 241 , effectively limiting any horizontal air movement to the computer servers inside the cabinets 240 . Specifically, lightweight filler panels installed above the cabinets 240 serve this purpose. This is another key to efficient air cooling, avoiding any mixture of cold and hot air outside of computer cabinets 240 . Inside the cabinets 240 themselves, depending on their design, some weather striping materials can also be used to fill smaller holes.
Once in the hot-aisle 241 , the air is free to rise through the gratings to the exhaust plenum 277 where it is either recirculated downward through the mixing dampers 275 and mixing plenum 236 , or exhausted upward through the exhaust vents 274 , depending on the modes of operation previously described.
Notably, the cooling system of the present embodiment of the module 200 can be built from standardized industrial parts readily available and manufactured in large quantities at low cost. Its global efficiency stems from the use of large capacity and high efficiency fans 237 and coils 222 that can be made much more efficient than their smaller counterparts usually found in conventional computing room air conditioner (CRAC) units. Moreover, the whole module 200 can be assembled rapidly from manufactured parts using well known and mastered metal structure building techniques. External party walls and weight bearing structures of modules 200 can be designed so that a new module 200 can attach to an existing one. Similarly, corridors 310 and 320 can be designed in a modular fashion so that new sections can be added with new modules 200 .
Furthermore, each module 200 comprises its own electrical systems, complete with voltage transformations, switch gear protection, and UPS 217 , possibly in 1n, n+1 or 2n redundant configurations. The ability to regroup all mechanical and electrical systems in a single autonomous module 200 is not only cost effective, it is scalable and flexible. A module operator can customize the capacity and resiliency of his module 200 to satisfy the specific needs of his users, without affecting the operations of other modules 200 . For instance, some modules 200 could operate with either no, partial, or full UPS protection, with or without redundancy. A priori decisions need not be taken for the whole site, nor do power density zones need to be defined. Decisions can be postponed to time of deployment, one module 200 at a time, or in blocks of multiple modules 200 . Modules 200 can be built on-demand. Upgrades of existing modules 200 are also feasible without affecting the operations of others. For instance, transformers could be upgraded to change from a 1n configuration to an n+1 configuration, or a UPS could be added, or support extended, if needs evolve over time.
Power distribution to computer cabinets is also flexible. It can rely on different technologies like classical breaker panels, busbars, or in-row PDU cabinets. Again, the choice need not be taken a priori for the whole site, but can be postponed to deployment time. The modularity of the module 200 allows for cost-effective and resilient evolution of the data center complex 10 over time.
The problem of cooling the heat dissipation of electrical components within the module 200 is also addressed by placing these components inside the cooling system, which is both a cost-effective and energy efficient solution. It then becomes a non-issue. The same is true for the control systems that include fan drives, valve controls, temperature sensors, differential pressure sensors, humidity sensors and controls, fire detection and protection, and access controls.
Referring to FIG. 7 , the deployment method for a large scale data center complex 10 is described by a flowchart. The method bootstraps (at 701 ) by constructing the central facility building 100 for housing the main power and cooling infrastructures that are shared by all modules 200 . This initial facility 100 is essentially an empty shell built on a concrete slab. It has some office space for administration, security, and maintenance staff, but most of its footprint is typically of low cost warehouse type. It must generally be sized according to the expected maximum power capacity of the whole data center complex 10 . Then, the corresponding medium or high voltage power feeds from the utility company must be installed with adequate voltage transformation, switch gears, and protection systems. If possible, this step shall be phased to minimize initial investments. The important thing is to have enough switch gear to make sure that additional power capacity can be added without having to interrupt services to existing modules 200 .
Backup generators and chillers modules should generally be installed one by one, as user needs evolve, maximizing ROI. Building modules 200 requires a concrete slab with strong foundations because of the weight of the computing machinery. As building these foundations may take a somewhat long lead time, especially for locations where the ground freezes during winter, it may be wise to anticipate user needs and build them well in advance for at least several (e.g. 4 ) modules 200 , including access corridors and passageways 310 and 320 . Obviously, this number can be increased if rapidly changing user needs are expected. The last step of this initial work is to build and setup the first module 200 to address the initial user needs. Again, if these needs are initially greater, the number of initial modules 200 should be augmented accordingly.
Afterward, user needs are constantly assessed (at 702 ) and if no longer fulfilled, a new module 200 is ordered, factory built and assembled on existing foundations (at 705 ). If no foundations are available (at 703 ), or if not enough of them are currently available to address the expected short term needs, then new foundations are built in increments of typically 4 or more (at 704 ). If medium voltage power or cooling capacity is short in the central facility 100 (at 706 ), but space and energy is still available (at 707 ), then new power and/or cooling modules are added to the main building 100 (at 708 ). Otherwise, if power and cooling capacity for the new modules 200 is short and space or energy is exhausted, then the site has reached its capacity and a new data center complex 10 must be built on a new site.
Referring to FIG. 8 a , the hybrid-loop control method 800 for cooling a module 200 is described with the help of a flowchart. This method 800 applies independently for each of the two cooling subsystems in the module 200 . The method starts (at 801 ) by initially fully opening the intake and exhaust dampers 276 and 278 , and fully closing the mixing dampers 275 . The chilled-water valve is also initially closed so that no water is flowing through the coils 222 . Finally, the humidifiers 224 are also initially shutoff.
Then, the method 800 enters a loop where outside air conditions are first evaluated. If temperature or humidity are out of limits (“yes” branch at 802 ), then the system may no longer operate in hybrid-loop and is automatically switched to closed-loop operation (see 900 of FIG. 9 ). Indeed, when the outside temperature nears the set-point temperature for the cold air plenum, the system can no longer operate in hybrid-loop in any practical way, so it reverts to closed loop operations. The decision can be implemented using either the outside dry bulb temperature or the more precise air enthalpy. If the outside conditions are favorable (“no” branch at 802 ), then the process continues by measuring the differential pressure on all floors 230 , between the cold and hot aisles 239 and 241 , for all cabinet rows 240 . The lowest measurement is kept and used to adjust the fan speed (at 805 ) if the pressure is determined to be out of limits (“yes” branch at 804 ). The acceptable range of differential pressure is between two small positive values. In the case where the cold-aisles 239 are maintained at temperatures below 20 degrees Celsius, the lower end of this range should be approximately zero; if the cold-aisle 239 is operated at higher temperature, it may need to be somewhat above zero to maintain a more aggressive minimum differential pressure. The fan speed adjustment method uses standard control algorithms for this purpose.
The next step is to regulate the temperature of the cold-aisles 239 if it is outside of the preset limits (at 806 ). The temperature is measured at the output of the cooling subsystem in the central cold air plenum 216 , below the first computing level 230 . Four variables can be controlled to achieve temperature regulation: the flow of water in the coils 222 , and the flow of air in the intake, exhaust, and mixing dampers 276 , 278 and 275 respectively (at 807 ).
Referring to FIG. 8 b , the method performed at 807 for adjusting the dampers and water flow is illustrated with a flowchart. When the current cold-aisle 239 temperature is too cold (“too cold” branch at 810 ), the method uses a strategy that prioritize the variables in the following order: water flow, mixing airflow, exhaust airflow, and intake airflow. If water is currently flowing, but not being reused by the central facility 100 (“yes” branch at 819 ), then its flow is decreased ( 820 ) to maximize the use of the air-side economizer cycle (which is the general objective of the hybrid-loop operation). Otherwise (“no” branch at 819 ), either no water is flowing, in which case flow cannot be reduced, or water is flowing, but needed by the central facility 100 for useful energy reuse. At this point, some warm air from the exhaust plenum 277 must be recirculated to further preheat the air in the mixing plenum 236 . If the mixing dampers 275 are not yet fully opened (“no” branch at 821 ), then it is opened some more to increase air mixing (at 822 ). In this way, more of the warm air in the exhaust plenum 277 is mixed with the external cold air to raise the air temperature of the input plenum 218 . On the contrary, if the mixing dampers 275 are already fully opened (“yes” branch at 821 ), then it is necessary to act on the exhaust dampers 278 by decreasing the flow of air that can exit the module 200 (at 824 ). In this way, more of the exhaust plenum air can mix with the outside air to raise the temperature in the input plenum 218 . In the extreme case, the exhaust dampers 278 are fully closed (“yes” branch at 823 ) and all of the warm hot-aisle 241 air is recirculated. When this happens, there is a possibility that some of this warm air under pressure will exit through the intake vent 272 instead of being sucked downward in the mixing plenum 236 , so the intake damper 276 cross-section needs to be decreased (at 825 ) to create a restriction that will force all the mixed air to flow downwards. It is not possible that the intake dampers 276 fully close unless no heat is dissipated by the computing machinery.
If the cold-aisle 239 temperature is too warm (“too warm” branch at 810 ), then the strategy is to prioritize the control variables in the reverse order: intake airflow, exhaust airflow, mixing airflow, and water flow, assuming that water is currently not being reused by the central facility (“no” branch at 811 ). If the intake dampers 276 are not fully opened (“no” branch at 812 ), then they should be opened some more to increased the intake airflow (at 813 ) and allow the possibility for more cold air to enter. Otherwise, they are already fully opened (“yes” branch at 812 ) and it is the exhaust dampers 278 that need to be opened to allow increased air exhaust (at 815 ) and, thus, increased air exchange with the outside. Otherwise, both intake and exhaust dampers 276 and 278 are fully opened, and it is the mixer dampers 275 that need to be closed some more if it is not already fully closed (“no” branch at 816 ), to decrease air mixing (at 817 ) and reduce the warming of the outside air. Otherwise, if the mixing dampers 275 are fully opened (“yes” branch at 816 ), or if the water is currently being reused by the central facility 100 (“yes” branch at 811 ), then the coils 222 need to absorb more heat by increasing their water flow (at 818 ).
Back to FIG. 8 a , the next step is adjusting the humidifier output (at 809 ) if the relative humidity in the cold air plenum 216 is out of limits (“yes” branch at 808 ) for normal operations of the computer servers, as specified by the computer manufacturers. The method for making this adjustment again uses standard algorithms. After this step, the process starts over by checking repeatedly outside air conditions, differential pressure, cold air plenum temperature, and humidity, and by making adjustments, whenever necessary.
The humidifiers increase relative humidity, essentially when the outside air temperature is very cold, and thus too dry once it has been warmed to its set-point temperature. For this purpose, the humidifiers 224 vaporize demineralized water using an efficient adiabatic mechanism. During the summer time, the relative humidity inside the module 200 can also become too high if the outside air is too humid. In those cases, however, the system will tend to switch to closed-loop operations, because the air enthalpy probably makes the air-side economizer cycle counterproductive. In any case, the excessive humidity will be removed by the cooling coils 222 through condensation.
Referring to FIG. 9 , the closed-loop control method 900 for cooling the module 200 is described with the help of a flowchart. The closed-loop method 900 is similar to the hybrid-loop one, but simpler because the temperature regulation has a single variable to work with: the flow of chilled-water in the coils 222 . The method 900 starts by fully closing the intake and exhaust dampers 276 and 278 , and fully opening the mixing dampers 275 so that all the air in the exhaust plenum 277 is recirculating into the input plenum 218 . The chilled-water valve is also initially closed so that no water is flowing through the coils 222 , and the humidifiers 224 are shutoff.
Then, the method enters a loop where outside air conditions are first evaluated. If temperature and humidity are within limits (“yes” branch at 902 ), then the system can switch back to hybrid-loop operations using the air-side economizer cycle. It should be noted here that the outside condition limits for switching from closed-loop to hybrid-loop are not necessarily the same as the one for switching from hybrid-loop to closed-loop. Some hysteresis should be used so that the system does not oscillate between the two modes of operation. If outside conditions are unfavorable (“no” branch at 902 ), then the method continues by measuring the differential pressure on all floors, between the cold and hot aisles 239 and 241 , on both sides of the cabinet rows 240 . The lowest measurement is kept and used to adjust the fan speed (at 904 ) if the differential pressure is determined to be out of limits (“yes” branch at 903 ). The acceptable range of differential pressure is between two small positive values. In the case where the cold-aisle 239 is maintained at temperatures below 20 degrees Celsius, the lower end of this range should be approximately zero; if the cold-aisles 239 are operated at higher temperature, it may need to be somewhat above zero to maintain a more aggressive minimum differential pressure. The speed adjustment method uses standard control algorithms for this purpose.
The next step is to regulate the temperature of the cold-aisle 239 by controlling the flow of water in the coils 222 . The temperature is measured at the output of the cooling subsystem in the cold air central plenum 216 . When the current temperature is out of limits (“yes” branch at 905 ), the method simply adjusts the water flow (at 906 ) in the coils 222 using standard control algorithms for this purpose.
The final step is adjusting the humidifier output (at 908 ) if the relative humidity in the cold air plenum 216 is out of limit (“yes” branch at 907 ) for normal operations of servers, as specified by the computer manufacturers. The method for making this adjustment again uses standard control algorithms. After this step, the process starts over by checking repeatedly outside air conditions, differential pressure, temperature, and humidity, and by making adjustments, whenever necessary.
While illustrative and presently preferred embodiments of the invention have been described in detail hereinabove, it is to be understood that the inventive concepts may be otherwise variously embodied and employed and that the appended claims are intended to be construed to include such variations except insofar as limited by the prior art. | A data center module is a data center that can be prefabricated using generally standardized off-the-shelf components, and quickly assembled on a collocation site where a shared central facility is provided. The data center module is typically configured to be deployed with other identical data center modules around the central facility both in side-to-side and/or in back-to-back juxtapositions, typically without the need for interleaving space between adjacent modules in order to maximize real estate use. Each data center module typically comprises harden party walls, several floors for accommodating all the necessary electrical and cooling subsystems and for accommodating all the computing machinery (e.g. servers). Though all the data center modules share similar physical configuration, each data center module can be independently customized and operated to accommodate different needs. Each data center module also incorporates a highly efficient hybrid cooling system that can benefit from both air-side and water-side economizers. | 7 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims priority to German application DE 10 2004 048875, filed Oct. 7, 2004.
FIELD OF THE INVENTION
The present invention relates to a novel process for preparing cyclic ketones such as alkyl cyclopentanone-2-carboxylates. The substances obtained in this way are used as basic building blocks for pharmaceuticals and crop protection agents, as fine chemicals, for the surface coatings industry, etc.
BACKGROUND OF THE INVENTION
The intramolecular condensation reaction named after Dieckmann (Ber. Dtsch. Chem. Ges. 1894 (27) 965, Liebigs Ann. 1901 (317) 27) is known. For example, the Dieckmann condensation of dialkyl adipates leads to alkyl cyclopentanone-2-carboxylates. The process is based on a condensation reaction in which the respective alcohol is liberated:
In these processes, the alkali metal salt or the alkaline earth metal salt of the desired compound is prepared with virtually quantitative conversion and selectivity and this salt is worked up under acid conditions in a further step. Many attempts to optimize the procedure and the yield of this reaction have been discussed in the literature. These relate to both the condensation agent to be used and the process methodology and solvents used.
For example, the cyclization of adipic esters by reaction with stoichiometric amounts of a strong Lewis acid (e.g. AlCl 3 , TiCl 2 (OTf) 2 ) and a base (e.g. NEt 3 ) as condensation agent has been described (e.g. Pecanha et al., Quim. Nova 20 (1997) 435; Tanabe et al., Chem. Lett. (1986) 1813). Here, the reaction takes place in solution in good yields, but stoichiometric amounts of Lewis acid and base (e.g. triethylamine) have to be used. In the subsequent aqueous work-up, the Lewis acid used is completely hydrolysed, which is undesirable from economic and ecological points of view.
In addition, many processes which bring about the cyclization by means of a strong base as condensation agent have been described. Suitable bases are, for example, alkali metals (e.g. Pinkney, Org. Synth. 1937 (17) 32), metal hydrides (e.g. Bloomfield et al., Tetrahedron Lett. 1964, 2273) or metal amides (e.g. Bouveault et al., Compt. Rend. 146 (1908) 138).
It has been found to be particularly useful to use alkoxides, in particular alkoxides of the alkali metals and alkaline earth metals, as bases (e.g. sodium ethoxide, Reed et al. J. Chem. Soc. 1954, 2148, or magnesium ethoxide, Laukkanen, Chem. Ber. 1957 (31) 124). The alkoxide is usually introduced into the reaction as a solution in the corresponding alcohol. To avoid transesterification of the starting material for the reaction or the reaction product by the alkoxide used or the alcohol used, it is usual to employ materials having an identical substitution pattern for the Dieckmann cyclization. (Methoxides in methanol for the cyclization of methyl esters, ethoxides in ethanol for the cyclization of ethyl esters, etc.). The alkoxides required are obtained either by reaction of the corresponding metal with the alcohol or by dewatering of alcoholic sodium hydroxide or potassium hydroxide.
Since Dieckmann reactions are equilibrium reactions, it is necessary to remove the alcohol liberated during the reaction and also the alcohol used as solvent quantitatively in order to achieve a quantitative conversion. A Dieckmann reaction is therefore usually carried out in nonpolar solvents such as toluene or xylene and the alcohol is distilled off.
The literature methods for Dieckmann cyclization using alkoxides in nonpolar solvents have various disadvantages for economical industrial use. A particular problem is that a viscous suspension comprising the starting materials for the reaction, the salt of the reaction product and the solvent is formed during the reaction and this can be stirred only with great difficulty from an industrial point of view. Only a low space-time yield can be achieved by means of this reaction, since it has to be carried out in a very dilute suspension which typically comprises only about 10–20% by weight of reactants and 80–90% by weight of solvent in order for the suspension to remain stirrable.
Furthermore, owing to the high viscosity of the mixture, it is usually not possible to bring about complete conversion, i.e. 100% reaction of the adipic ester, in an acceptable time. In this case, a product which still contains amounts of starting material is obtained after hydrolysis of the reaction mixture. This starting material can be separated off from the desired cyclic alkyl ketonecarboxylate by distillation only with great difficulty, since the substances have similar boiling points.
The use of various solvents which reduce the viscosity of the reaction mixture and are said to enable the Dieckmann cyclization to be carried out more easily as a result has been described.
Cassebaum et al. (DD-A 085560 (1971); Z. Chem. 1971 (11) 14) describe a process in which the reaction with sodium ethoxide as base is carried out in a solvent mixture of o-dichlorobenzene and dimethylformamide.
Richter Gedeon (HU-A 173512, 1978) likewise describe a process in which dipolar, aprotic solvents (e.g. dimethylformamide) are used for Dieckmann reactions.
Kao Corp (JP-A 9183755, 1997) carries out the reaction in solvent mixtures of aromatic organic solvents (e.g. toluene, xylene) and in tertiary alcohols (e.g. tert-butanol, amyl alcohol). The corresponding tertiary alkoxides as condensation agents are produced by reaction of the tertiary alcohol with sodium or sodium hydride.
Processes in the presence of a solvent have various disadvantages. The separation and recovery of the alcohol from the solvents used is complicated. Water present in the solvents used reacts with the strong bases used and decomposes them. Polar solvents or solvent mixtures are somewhat expensive and difficult to regenerate. They are completely or partially miscible with water, so that the polar solvent or the polar components of the solvent mixture are dissolved in the aqueous phase during the work-up of the reaction mixture as a result of acid, aqueous hydrolysis. The polar solvents can be recovered from the aqueous phase only with great difficulty. In addition, proportions of the reaction product can also be carried together with the polar solvent into the aqueous phase. When highly polar solvents or solvent mixtures are used, no phase separation occurs on hydrolysis, but instead a uniform water/solvent/product phase which can be worked up only with great difficulty is formed. The extraction with a nonpolar solvent which is necessary to recover the product from the aqueous phase and the complicated recovery of the highly polar solvent from the aqueous phase are substantial disadvantages of the methodology described.
Processes which do not use an additional solvent are therefore advantageous. VEB Fahlberg List (DE-A 2055009 (1972)) describe a process in which the reaction is carried out exclusively in the alcohol used for the synthesis of the condensation agent. For example, magnesium powder is dissolved in an excess of ethanol for the synthesis of ethyl cyclopentanone-2-carboxylate. The magnesium ethoxide formed is admixed with diethyl adipate and ethanol is distilled off, forming a resin-like mass.
This process has various disadvantages. The use of a solvent continues to be necessary. The quantitative removal of the alcohol necessary for a quantitative conversion is possible only under drastic conditions; the mixture is heated to about 220° C. for 1¾ to 2½ hours at a batch size of 1.6 mol. This procedure is unsuitable for production on an industrial scale. In the further course of the process disclosed, the resin-like mass has to be dissolved in benzene before hydrolysis. The use of additional solvents is therefore still necessary during the course of the process. Only 90% of the benzene used can be recovered.
Processes in which alcohol for dissolving the condensation agent can also be dispensed with are therefore particularly advantageous. Toda et al. (J. Chem. Soc., Perkin Trans. 1, 1998/3521) describe a method in which an alcohol for dissolving the alkoxide used is also dispensed with. Here, the dialkyl adipate is triturated with a solid alkali metal alkoxide in a pestle and mortar. The reaction product is set free from the salt by addition of p-toluenesulphonic acid. Interestingly, a quantitative conversion is not achieved in this example. A yield of 61% is reported in the reaction of diethyl adipate with sodium methoxide. A higher yield (82%) is reported when using potassium tert-butoxide as condensation agent.
This method has various disadvantages for use on an industrial scale. Costly condensation agents (e.g. sodium ethoxide) give only moderate yields. Based on the size of the batches, the specific mechanical energy introduced via the pestle is considerable.
It was therefore an object of the invention to find a technically simple process which allows the preparation of alkyl cyclopentanone-2-carboxylates with a low economic outlay while completely dispensing with solvents and at the same time resulting in complete reaction of the alkyl adipate.
SUMMARY OF THE INVENTION
This object is achieved by the process of the invention. It has surprisingly been found that complete conversion can be achieved in the absence of a solvent in a solid-state reactor or in a high-viscosity reactor.
The present invention therefore provides a process for preparing cyclic ketones of the general formula (I),
where
X is an electron-pulling group, R 1 and R 2 are each, independently of one another, H, C 1 –C 20 -(cyclo)alkyl, C 6 –C 24 -aryl, C 1 –C 20 -(cyclo)alkyl ester or C 1 –C 20 -(cyclo)alkylamide, C 6 –C 24 -aryl ester or C 6 –C 24 -arylamide, a mixed aliphatic/aromatic radical having from 1 to 24 carbon atoms, which can also be part of a 4- to 6-membered ring,
characterized in that a metal base is reacted with a compound of the general formula (II)
where, independently of one another, the radicals
R 1 and R 2 are as defined above, R 3 is an alkyl or aryl radical and X is an electron-pulling group,
in a solid-state reactor or high-viscosity reactor without additional solvents being used.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
As used herein, as used in the examples or unless otherwise expressly specified, all numbers may be read as if prefaced by the word “about”, even if the term does not expressly appear. Also, any numerical range recited herein is intended to include all sub-ranges subsumed therein.
The process of the invention is advantageously carried out using solid-state reactors, high-viscosity reactors or mixing kneaders which have sufficient kneading power and are provided with a facility for taking off the volatile reaction products. In addition, machines which can be evacuated and/or can additionally be heated are advantageous. The space-time yield is significantly increased by evacuation and heating and the resulting accelerated removal of the volatiles, which leads to a significant improvement in the economics. The mixing action and the input of mechanical energy in these types of apparatus are sufficient to bring about complete conversion.
The process of the invention can be carried out in single-shaft or multishaft machines. The single-shaft machines include, for example, mixing kneaders, blade dryers or comparable apparatuses which ensure homogeneous mixing of the starting materials and thus complete conversion. Examples of such apparatuses are described, for example, in EP-A 0 729 780 (Draiswerke), EP-A 0 611 937 (Draiswerke), DE-A 19 747 218 (Lödige), EP-A 0 304 925 (List).
The process of the invention is particularly advantageously carried out in multishaft mixing kneaders or high-viscosity reactors. The shafts are provided with mixing elements which can intermesh and thus ensure some self-cleaning action. The mixing or kneading shafts can be corotating or counterrotating. The rotational movement of the shafts and the kneading elements affixed thereto ensures the introduction of sufficient energy to achieve good mixing and thus complete conversion. Examples of partially self-cleaning machines may be found, for-example, in EP-A 0 329 092 (List) and EP-A 0 517 068 (List). An example of a fully self-cleaning machine is described in EPA 0 460 466 (Bayer).
The machines mentioned additionally have a large free volume which is necessary for effective removal of the volatile reaction products and thus for a good space-time yield. The apparatuses mentioned can, depending on configuration, be operated batchwise or continuously. For continuous operation, appropriate feed and discharge facilities need to be provided, as described, for example, in WO 02/20885.
The process of the invention can likewise advantageously be carried out in a multiscrew extruder. Multiscrew extruders have an extremely good mixing action and a good self-cleaning action. Corotating or counterrotating multiscrew extruders are known to those skilled in the art as machines for the reaction, plasticization and degassing of paste-like or high-viscosity media or for the transport of solids. Extruders having two or more screws are suitable. Planetary-gear extruders can also be used (e.g. DE-A 10 054 854, Entex). Frequent and effective renewal of the surface in an extruder, which ensures good mass transfer and thus rapid removal of the volatile constituents, likewise has a positive effect on the process.
In a high-viscosity reactor, maximum residence times of 30 minutes and more can be achieved, while economical residence times in an extruder are in the range from 10 seconds to 10 minutes. The way in which the process is carried out, determined by temperature and pressure, has to be matched to the circumstances of the machines. The relationship between residence time, mass transfer, temperature and pressure is known to those skilled in the art.
Any 5–7 cycloketones can be prepared by the process of the invention.
The process of the invention is suitable for producing CH-acid cycloketones of the general formula (I),
where
X is an electron-pulling group (carboxylic ester or nitrile), R 1 and R 2 are each, independently of one another, H, C 1 –C 20 -(cyclo)alkyl, C 6 –C 24 -aryl, C 1 –C 20 -(cyclo)alkyl ester or C 1 –C 20 -(cyclo)alkylamide, C 6 –C 24 -aryl ester or C 6 –C 24 -arylamide, a mixed aliphatic/aromatic radical having from 1 to 24 carbon atoms, which can also be part of a 4- to 8-membered ring, n is an integer from 0 to 3,
with complete conversion of the parent ester component.
The electron-pulling group X can be any substituent which leads to CH acidity of the hydrogen in the a position. It can be, for example, an ester group, a nitrile group or a carbonyl group. Preference is given to ester groups, particularly preferably methyl carboxylate and ethyl carboxylate groups.
Also suitable are compounds of the general formula (I) whose ring likewise contains heteroatoms such as oxygen, sulphur or nitrogen atoms.
The activated cyclic ketone of the formula (I) preferably has a ring size of 5 (n=1) or 6 (n=2).
Preferred compounds of the general formula (I) are methyl cyclopentanone-2-carboxylate and ethyl cyclopentanone-2-carboxylate, cyclopentanone-2-carbonitrile, methyl cyclohexanone-2-carboxylate and ethyl cyclohexanone-2-carboxylate and 2-methylcarbonylcyclopentanone. Particular preference is given to methyl cyclopentanone-2-carboxylate and ethyl cyclopentanone-2-carboxylate and also methyl cyclohexanone-2-carboxylate and ethyl cyclohexanone-2-carboxylate.
The cyclopentanone systems can easily be obtained industrially by the abovementioned Dieckmann condensation of dimethyl adipate or diethyl adipate.
The invention is described by the following examples.
EXAMPLES
Preparation of Cyclic 1,3-diketo Compounds
Example 1
The process was carried out in a high-viscosity reactor model CRP 2,5 Batch from List AG. The high-viscosity reactor is a machine having two horizontal corotating mixing shafts. Kneading devices which intermesh and thus ensure rapid and homogeneous mixing are located on the shafts. In addition, the machine has a discharge screw by means of which the product can be conveyed out of the reaction chamber. It can be operated continuously or batchwise. The reactor has a free volume of about 2.5 l. The reaction chamber of the machine can be heated. Volatile constituents can be taken off via a vent. 1336 g of diethyl adipate and 472 g of sodium ethoxide were placed in the high-viscosity reactor. After start-up of the kneader and commencement of mixing of the starting materials a viscous mass was immediately formed. While kneading slowly, the temperature was slowly increased to 120° C. A vacuum of 10 mbar was slowly built up. The temperature of 120° C. was reached after about 15 minutes. Slow kneading was then continued at a temperature of 120° C. for 30 minutes until a pulverized white solid had been obtained. The powder formed was discharged by means of a transport screw and subsequently hydrolysed using half-strength sulphuric acid. Phase separation and distillation at 120° C./10 mbar gave 1021 g of ethyl cyclopentanone-2-carboxylate, viz. about 99% of theory. Diethyl adipate could no longer be detected.
Example 2
The process was carried out in a corotating twin-shaft extruder model ZSK34 having a shaft diameter of 34 mm. The process section of the machine had a length of 1560 mm. The machine was provided with an opening for the introduction of solids. The liquid was introduced via a drilled hole in the barrel. Mixing of the components is effected by the kneading elements located on the shaft. The volatile reaction products were taken off via an open venting facility. 1.31 kg/h of sodium methoxide as powder and 3.69 kg/h of diethyl adipate as liquid were metered into the machine. The rotational speed of the machine was about 60 l/min. The mixture was heated to about 150° C. by means of the barrel heating. At the end of the machine, a crumbly white solid was discharged. After acidification, aqueous work-up and extraction with an organic solvent (toluene), no starting material in the form of diethyl adipate, monomethyl adipate or adipic acid could be detected. Only ethyl cyclopentanone-2-carboxylate was found. The yield based on diethyl adipate was quantitative.
Although the invention has been described in detail in the foregoing for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims. | The present invention provides a process for preparing cyclic 1,3-keto esters in the absence of solvent, using solid-state or high viscosity reactors. | 2 |
FIELD OF THE INVENTION
[0001] The present invention relates to a light guide film of a light emitting diode (LED) backlight unit, and, more particularly, to a light guide film of an LED backlight unit, which has a plurality of grooves carved into an incident plane of the light guide film to increase an incidence angle of which light can be transmitted through the light guide film.
BACKGROUND OF THE INVENTION
[0002] Typically, a liquid crystal display (LCD) for handheld and notebook devices generally employs at least one lateral light emitting diode (LED) as a light source of a backlight unit. Such a lateral LED is generally provided to the backlight unit as shown in FIG. 1 of Yang U.S. Pat. No. 7,350,958.
[0003] Referring to FIG. 1 , the backlight unit 10 comprises a planar light guide film 20 disposed on a substrate 12 , and a plurality of lateral LEDs 30 (only one lateral LED is shown in FIG. 1 ) disposed in an array on a lateral side of the light guide film 20 . Light L entering the light guide film 20 from the LED 30 is reflected upwardly by a minute reflection pattern 22 and a reflection sheet (not shown) positioned on the bottom of the light guide film 20 , and exits from the light guide film 20 , providing back light to an LCD panel 40 above the light guide film 20 . Such a backlight unit 20 suffers from a problem as shown in FIG. 2 when light is incident on the light guide film 20 from the LED 30 .
[0004] As shown in FIG. 2 , light L emitted from each LED 30 is refracted toward the light guide film 20 by a predetermined angle θ due to difference in refractive index between media according to Snell's Law when the light L enters the light guide film 20 . In other words, even though the light L is emitted at a beam angle of α 1 from the LED 30 , it is incident on the light guide film 20 at an incidence angle of α 2 less than α 1 . In FIG. 3 , such an incidence profile of light L is shown. Therefore, there is a problem of increasing the length (l) of a combined region where beams of light L entered the light guide film 20 from the respective LEDs 30 are combined. In addition, light spots H also called “hot spots” and dark spots D are alternately formed in the region corresponding to the length (l) on the incident plane of the light guide film 20 . Each of the light spots H is formed at a location facing the LED 30 , and each of the dark spots D is formed between the light spots H.
[0005] Since the alternately formed light and dark spots are not desirable for the light guide film, they should be minimized and the length (l) should be shortened as much as possible. For this purpose, it is necessary to increase an angle of light entering the light guide film, that is, an incidence angle of light.
[0006] For this purpose, it is suggested to form protrusions on the input surface of the light guide film as shown in FIG. 4 . Specifically, a plurality of fine prism-shaped structures 24 or arc-shaped structures (not shown) are formed on a light input surface of a light guide film 20 A and light L enters the light guide film at an incidence angle α 3 substantially equal to an orientation angle α 1 of light emitted from a focal point F of a light source. Thus, if orientation angles al of light beams emitted from the focal point F of the light source are identical, the light L enters the light guide film at an incidence angle α 3 wider than the case of FIGS. 2 and 3 . However, with this solution, there is some secondary light collimation where the light rays are refracted by the wall of the adjacent prism or arc-shaped structure as shown in FIG. 4 . Secondary light collimation from the walls of the adjacent prism structure turns the light ray back on-axis providing less diffusion of the light from the light source as shown in FIG. 4 . Thus the continuous prism- or arc-shaped structures on the input surface have limited light diffusing capability.
[0007] Therefore an improved input edge design is needed to provide a more uniform surface illumination of the light guide film without sacrificing the efficiency of the backlight system.
SUMMARY OF THE INVENTION
[0008] The present invention provides a planar light guide film for a backlight unit having at least one point light source, the light guide film comprising: a light input surface for receiving light from the point light source; a light redirecting surface for redirecting light received from the light input surface; a light output surface for outputting at least the light redirected from the light redirecting surface; wherein the light input surface further comprises a composite lens structure having a circular tip segment with a first contact angle, and a first and second elliptical base segments with a second contact angle, the second contact angle being greater than the first contact angle and the second contact angle being equal to each other; and
[0000] wherein the circular tip segment satisfies the following equation:
[0000] y 1 =a 1 +√{square root over (( r 1 2 −x 2 ))}
[0000] and the elliptical base segments satisfies the following equations:
[0000] y 4 =d 4 +b 4 ×√{square root over ((1−(( x+c 4 )/ a 4 ) 2 )}
[0000] y 5 =d 5 +b 5 ×√{square root over ((1−(( x−c 5 )/ a 5 ) 2 )}
[0009] In addition, the invention further provides a planar light guide film for a backlight unit having at least one point light source, the light guide film comprising: a light input surface for receiving light from the point light source; a light redirecting surface for redirecting light received from the light input surface; a light output surface for outputting at least the light redirected from the light redirecting surface; wherein the light input surface further comprises a composite lens structure having gaps there between, the lens structure having a circular tip segment with a first contact angle, and a first and second elliptical base segments with a second contact angle, the second contact angle being greater than the first contact angle and the second contact angle being equal to each other; and
[0000] wherein the circular tip segment satisfies the following equation:
[0000] y 1 =a 1 +√{square root over (( r 1 2 −x 2 ))}
[0000] and the elliptical base segments satisfies the following equations:
[0000] y 4 =d 4 +b 4 ×√{square root over ((1−(( x+c 4 )/ a 4 ) 2 )}
[0000] y 5 =d 5 +b 5 ×√{square root over ((1−(( x−c 5 )/ a 5 ) 2 )}
[0010] Further, the invention provides a planar light guide film for a backlight unit having at least one point light source, the light guide film comprising: a light input surface for receiving light from the point light source; a light redirecting surface for redirecting light received from the light input surface; a light output surface for outputting at least the light redirected from the light redirecting surface; wherein the light input surface further comprises a serrated lens structure that is provided only where the point light source is incident on the light input surface, the lens structure having a circular tip segment with a first contact angle, and a first and second elliptical base segments with a second contact angle, the second contact angle being greater than the first contact angle and the second contact angle being equal to each other; and
[0000] wherein the circular tip segment satisfies the following equation:
[0000] y 1 =a 1 +√{square root over (( r 1 2 −x 2 ))}
[0000] and the elliptical base segments satisfies the following equations:
[0000] y 4 =d 4 +b 4 ×√{square root over ((1−(( x+c 4 )/ a 4 ) 2 )}
[0000] y 5 =d 5 +b 5 ×√{square root over ((1−(( x−c 5 )/ a 5 ) 2 )}
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 shows a schematic diagram illustrating a conventional backlight module;
[0012] FIG. 2 shows a schematic diagram illustrating the distribution of bright/dark bands of a conventional light guide plate;
[0013] FIG. 3 shows a schematic diagram illustrating an embodiment of conventional light-diffusing structures;
[0014] FIG. 4 shows a schematic diagram illustrating another embodiment of conventional light-diffusing structures;
[0015] FIGS. 5 a and 5 b shows a schematic diagram illustrating a light guide film according to an embodiment of the invention;
[0016] FIG. 6 a - 6 c show schematic diagrams illustrating the various segments of the composite lens feature according to an embodiment of the invention;
[0017] FIGS. 7 a and 7 b show schematic diagrams illustrating the light diffusing capability of the composite lens feature with a gap between each adjacent feature;
[0018] FIG. 8 shows another embodiment of this invention;
[0019] FIGS. 9 a and 9 b show the luminance intensity at various distances from the light input surface for a circular or arc shaped input feature;
[0020] FIGS. 10 a and 10 b show the luminance intensity at various distances from the light input surface for a trapezoidal feature or feature with slanted sides; and
[0021] FIGS. 11 a and 11 b show the luminance intensity at various distances from the light input surface according to an embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0022] A light guide film in accordance with the present invention comprises a light output surface, a light redirecting surface and at least one light input surface that joins the light output surface and the light redirecting surface. The light input surface comprises a plurality of concave features consisting of a composite lens array. Each of the composite lenses is separated by a gap that is a flat surface perpendicular to the light output surface. The composite lenses and gaps are disposed along the light input surface, and extend from the output surface to the light redirecting surface. Each of the composite lenses has a symmetric cross-section consisting of a tip portion comprising a circular tip segment of a first contact angle and a base portion comprising two tilted elliptical base segments with a second contact angle, the second contact angle being greater than the first contact angle and where the contact angle for each of the two tilted elliptical base segments are equal.
[0023] According to the above embodiment, the geometrical profile of the composite lens allows for comparatively large light deflecting distances; that is, the composite lens structure has better light-diffusing capability. Thus, the distance between the point light source and the active area of the display can be shortened, and the dark spots between the point light sources can be minimized, with the brightness uniformity still being acceptable. The circular tip segment uniformly distributes the light in front of the discrete light source, typically a light emitting diode (LED). The two tilted elliptical base segments uniformly distribute the light between the LEDs. A smooth curvature of the circular tip segment and tilted elliptical base segments maximizes the uniformity of the light spatial distribution so that the light output is uniform. Further, it is also necessary that each two adjacent composite lens structures have a gap or flat therebetween so a greater degree of deflection on the propagation path of the incident light can be achieved to thereby increase the light-diffusing effect.
[0024] Referring to FIGS. 5 a and 5 b , a light guide film according to an embodiment of the invention is shown, wherein a planar light guide film 12 is used to receive and guide the light from at least one point light source (such as LEDs 14 shown in FIG. 5 a ). The side surface of the light guide film 12 next to the LED 14 forms a light input surface 12 a. The top surface of the light guide film 12 that makes an angle with the light input surface 12 a forms a light-emitting surface 12 b, and the bottom surface opposite the light-emitting surface 12 b forms a light-reflecting surface 12 c. The light-reflecting surface 12 c is comprised of a plurality of light reflecting structures. The light emitted from the LED 14 enters the light guide film 12 via the light input surface 12 a and propagates inside the light guide film 12 . Then, it is guided toward the light-emitting surface 12 b by the light-reflecting surface 12 c and finally exits the light guide film 12 through the light-emitting surface 12 b.
[0025] Further, a plurality of concave composite lens structures 16 are serrated on the edge of the light input surface 12 a, with their longitudinal directions being parallel to each other and having a gap (G) between each adjacent composite lens structure 16 . Referring now to FIGS. 6 a , 6 b and 6 c , the light input surface 12 a, facing the LED 14 , of the composite lens structure 16 has a circular tip segment 16 a, and two tilted elliptical base segments 16 b and 16 c, respectively. The circular tip segment 16 a of the concave composite lens structure 16 is the segment furthest from the light input surface 12 a. Although the composite lens features for the preferred embodiment of this invention are disposed in a concave direction on the light input surface, the composite lens may also be in a convex direction on the light input surface.
[0026] The length T 1 is the distance between the intersections of the extensions of the tangent at the top of the elliptical base segments 16 b and 16 c, and the tangent of the circular tip segment 16 a, where the tangent of the circular tip segment 16 a is parallel to the light input surface 12 a. The length T 2 is the total width of the circular tip segment 16 a taken where the circular tip segment 16 a intersects the two elliptical base segments 16 b and 16 c. Note, T 2 is parallel to T 1 . The contact angle A 1 is the contact angle of the circular tip segment 16 a. Contact angle A 1 is preferably greater than 0.1 degrees and less than or equal to 85 degrees. Referring now to FIG. 6 b , the gap G is the distance between each adjacent composite lens. Preferably, the gap G is less than or equal to 0.9 times the pitch P. The pitch P of the linear composite lens array 16 is the distance along the light input edge which includes the gap G distance and the total width B of the composite lens. Preferably the pitch P is greater than or equal to 5 micrometers and less than or equal to 1 millimeter (mm) The total height H of the feature is measured from the light input edge to the tangent of the circular tip segment 16 a. The total height H of the composite lens is greater than or equal to 3 micrometers and less than or equal to 1 millimeter. The light input surface 12 a will have a surface finish of 10 nanometers to 2 micrometers. The surface finish of the concave composite lens structures 16 can be the same or different than the gap G portion between the features.
[0027] Advantageously, the shape of an XY section of the circular tip segment 16 a satisfies the following expression (1):
[0000] y 1 =a 1 +√{square root over (( r 1 2 −x 2 ))} (1)
[0000] where the circular tip segment 16 a has a first radius r 1 . The first radius r 1 is defined as the quotient of half the distance T 1 divided by the tangent of half the contact angle A 1 . The value a 1 is defined as the total height H minus the radius r 1 of the circular tip segment 16 a. The value x is a value in the direction of the light input surface and is preferably set within the range of −r 1 ×sin(A 1 )≦x≦r 1 ×sin(A 1 ). The value y 1 is a value in the light propagation direction. Referring now to FIG. 6 c , the composite lens structure also comprises two tilted elliptical segments, namely a first elliptical base segment 16 b and a second elliptical base segment 16 c. Each elliptical base segment comprises two contact angles, a top contact angle and a bottom contact angle. The first elliptical base segment 16 b has a top contact angle A 41 and a bottom contact angle A 42 . The second elliptical base segment 16 c has a top contact angle A 51 and a bottom contact angle A 52 . The top contact angle A 41 is created by a tangent to the first elliptical base segment 16 b at the point where the circular tip segment 16 a and the first elliptical base segment 16 b intersect. The bottom contact angle A 42 is created by a tangent to the first elliptical base segment 16 b at the point where the first elliptical base segment 16 b intersects the light input surface 12 a. The top contact angle A 41 of the first elliptical base segment 16 b and the top contact angle A 51 of the second elliptical base segment 16 c are equal. The bottom contact angle A 42 of the first elliptical base segment 16 b and the bottom contact angle A 52 of the second elliptical base segment 16 c are equal. The contact angles for each of the two elliptical base segments 16 b and 16 c are larger than the contact angle A 1 of the circular tip segment 16 a.
[0028] Advantageously, the shape of an XY section of the elliptical base segments 16 b and 16 c as shown in FIG. 6 c satisfy the following expressions (2 and 3) respectively:
[0000]
y
4
=
d
4
+
b
4
×
(
1
-
(
(
x
+
c
4
)
/
a
4
)
2
(
2
)
y
5
=
d
5
+
b
5
×
(
1
-
(
(
x
-
c
5
)
/
a
5
)
2
Wherein
:
H
3
=
H
-
r
1
×
[
1
-
cos
(
A
1
)
]
B
=
P
-
G
a
4
=
ab
4
×
(
B
-
T
2
)
×
[
4
H
3
+
(
tan
(
A
41
)
+
tan
(
A
42
)
)
×
(
B
-
T
2
)
]
(
tan
(
A
41
)
+
tan
(
A
42
)
)
b
4
=
2
×
ab
4
×
H
3
×
[
H
3
×
(
tan
(
A
41
)
+
tan
(
A
42
)
)
+
tan
(
A
41
)
×
tan
(
A
42
)
×
(
B
-
T
2
)
]
(
tan
(
A
41
)
+
tan
(
A
42
)
)
where
:
ab
4
=
(
tan
(
A
41
)
+
tan
(
A
42
)
)
×
(
2
H
3
+
tan
(
A
41
)
×
(
B
-
T
2
)
)
×
(
2
H
3
+
tan
(
A
42
)
×
(
B
-
T
2
)
)
4
×
[
4
H
3
+
(
tan
(
A
41
)
+
tan
(
A
42
)
)
×
(
B
-
T
2
)
]
×
[
H
3
×
(
tan
(
A
41
)
+
tan
(
A
42
)
)
+
tan
(
A
41
)
×
tan
(
A
42
)
×
(
B
-
T
2
)
]
c
4
=
tan
(
A
41
)
×
⌊
2
H
3
×
B
+
tan
(
A
42
)
×
(
B
2
-
T
2
2
)
⌋
+
2
H
3
×
T
2
×
tan
(
A
42
)
4
×
{
tan
(
A
41
)
×
[
H
3
+
tan
(
A
42
)
×
(
B
-
T
2
)
]
+
H
3
×
tan
(
A
42
)
}
d
4
=
H
3
×
[
2
H
3
+
tan
(
A
41
)
×
(
B
-
T
2
)
]
4
H
3
+
(
tan
(
A
41
)
+
tan
(
A
42
)
)
×
(
B
-
T
2
)
(
3
)
[0029] Thus, the first elliptical base segment 16 b has a top contact angle A 41 and a bottom contact angle A 42 and the second elliptical base segment 16 c has a top contact angle A 51 and a bottom contact angle A 52 . Referencing FIGS. 6 a and 6 c , and equation 2, the height H 3 of the first elliptical base segment 16 b is equal to the total height H of the composite lens feature 16 minus the radius r 1 of the circular tip segment 16 a times the quantity 1 minus the cosine of contact angle A 1 of the circular tip segment 16 a. The total width B of the composite lens feature 16 is equal to the pitch P of the composite lens array minus the gap G distance. Preferably gap G is greater than 0 and less than or equal to 0.9 times the pitch P. The pitch P is preferably greater than or equal to 5 micrometers and less than or equal to 1 millimeter. The height of the second elliptical base segment 16 c is equal to the height H 3 of the first elliptical base segment 16 b.
[0030] The parameter a 4 is equal to the parameter ab 4 times the square root of the quotient of the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a times the quantity 4 times the height H 3 of the elliptical base segment 16 b plus the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by the quantity the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b.
[0031] The parameter b 4 is equal to 2 times the parameter ab 4 times the square root of the quotient of the quantity of the height H 3 of the first elliptical base segment 16 b times the quantity the height H 3 of the first elliptical base segment 16 b times the tangent contact angle A 41 of the top of the first elliptical base segment 16 b plus the tangent contact angle A 42 at the bottom of elliptical base segment 16 b plus the tangent contact angle A 41 times the tangent contact angle A 42 times the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by the quantity of tangent contact angle A 41 plus tangent contact angle A 42 .
[0032] The parameter ab 4 is equal to the quotient of the quantity the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the quantity twice the height H 3 of the first elliptical base segment 16 b plus the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a times the quantity twice the height H 3 of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by 4 times the following quantities the quantity the height H 3 of the first elliptical base segment 16 b times 4 plus the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a, plus the quantity the height H 3 of the first elliptical base segment 16 b times the quantity the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b plus the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b times the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the quantity times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a.
[0033] The parameter c 4 is equal to the quotient of the quantity the tangent contact angle A 41 at the top of the first elliptical base segment 16 b times the quantity twice the height H 3 of the first elliptical base segment 16 b times the total width B of the composite lens feature 16 plus the tangent contact angle A 42 times the quantity the total width B of the composite lens feature 16 squared minus the total width T 2 of the circular tip segment 16 a squared, that quantity plus twice the height H 3 of the first elliptical base segment 16 b times the total width T 2 of the circular tip segment 16 a times the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b divided by the tangent contact angle A 41 at the top of the first elliptical base segment 16 b times the quantity the height H 3 of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a plus quantity the height H 3 of the first elliptical base segment 16 b times the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b the quantities of the divisor times 4.
[0034] The parameter d 4 is equal to the quotient of the quantity twice the height H 3 of the first elliptical base segment 16 b plus the of tangent contact angle A 41 at the top of the first elliptical base segment 16 b times the quantity the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a, the previous quantities times the height H 3 of the first elliptical base segment 16 b divided by the height H 3 of the first elliptical base segment 16 b times 4 plus the quantity plus the tangent of contact angle A 41 at the top of the first elliptical base segment 16 b plus the tangent of contact angle A 42 at the bottom of the first elliptical base segment 16 b times the quantity the total width B of the composite lens feature 16 squared minus the total width T 2 of the circular tip segment 16 a.
[0035] The coordinate x is a value in the direction of the input edge or more specifically in the direction of the total width of the composite lens feature 16 and is preferably set within the range of −B/2≦x≦−T 2 /2 for the first elliptical base segment 16 b. The coordinate y 4 is a value in the light propagation direction.
[0036] Referencing FIGS. 6 a and 6 c , and equation 3, the height H 3 of the second elliptical base segment 16 c is equal the height of the first elliptical base segment 16 b. The total width B of the composite lens feature 16 is equal to the pitch P of the composite lens array minus the gap G distance. Preferably gap G is greater than 0 and less than or equal to 0.9 times the pitch P.
[0000]
a
5
=
ab
5
×
(
B
-
T
2
)
×
[
4
H
3
+
(
tan
(
A
51
)
+
tan
(
A
52
)
)
×
(
B
-
T
2
)
]
(
tan
(
A
51
)
+
tan
(
A
52
)
)
b
5
=
2
×
ab
5
×
H
3
×
[
H
3
×
(
tan
(
A
51
)
+
tan
(
A
52
)
)
+
tan
(
A
51
)
×
tan
(
A
52
)
×
(
B
-
T
2
)
]
(
tan
(
A
51
)
+
tan
(
A
52
)
)
where
:
ab
5
=
(
tan
(
A
51
)
+
tan
(
A
52
)
)
×
(
2
H
3
+
tan
(
A
51
)
×
(
B
-
T
2
)
)
×
(
2
H
3
+
tan
(
A
52
)
×
(
B
-
T
2
)
)
4
×
[
4
H
3
+
(
tan
(
A
51
)
+
tan
(
A
52
)
)
×
(
B
-
T
2
)
]
×
[
H
3
×
(
tan
(
A
51
)
+
tan
(
A
52
)
)
+
tan
(
A
51
)
×
tan
(
A
52
)
×
(
B
-
T
2
)
]
c
5
=
tan
(
A
51
)
×
⌊
2
H
3
×
B
+
tan
(
A
52
)
×
(
B
2
-
T
2
2
)
⌋
+
2
H
3
×
T
2
×
tan
(
A
52
)
4
×
{
tan
(
A
51
)
×
[
H
3
+
tan
(
A
52
)
×
(
B
-
T
2
)
]
×
H
3
×
tan
(
A
52
)
}
d
5
=
H
3
×
[
2
H
3
+
tan
(
A
51
)
×
(
B
-
T
2
)
]
4
H
3
+
(
tan
(
A
51
)
+
tan
(
A
52
)
)
×
(
B
-
T
2
)
[0037] The parameter a 5 is equal to the parameter ab 5 times the square root of the quotient of the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a times the quantity 4 times the height H 3 of the second elliptical base segment 16 c plus the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by the quantity the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c.
[0038] The parameter b 5 is equal to 2 times the parameter ab 5 times the square root of the quotient of the quantity of the height H 3 of the second elliptical base segment 16 c times the quantity the height H 3 of the second elliptical base segment 16 c times the tangent contact angle A 51 of the top of the second elliptical base segment 16 c plus the tangent contact angle A 52 at the bottom of elliptical base segment 16 c plus the tangent contact angle A 51 times the tangent contact angle A 42 times the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by the quantity of tangent contact angle A 51 plus tangent contact angle A 52 .
[0039] The parameter ab 5 is equal to the quotient of the quantity the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the quantity twice the height H 3 of the second elliptical base segment 16 c plus the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a times the quantity twice the height H 3 of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a divided by 4 times the following quantities the quantity the height H 3 of the second elliptical base segment 16 c times 4 plus the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a, plus the quantity the height H 3 of the second elliptical base segment 16 c times the quantity the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c plus the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c times the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the quantity times the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a.
[0040] The parameter c 5 is equal to the quotient of the quantity the tangent contact angle A 51 at the top of the second elliptical base segment 16 c times the quantity twice the height H 3 of the second elliptical base segment 16 c times the total width B of the composite lens feature 16 plus the tangent contact angle A 52 times the quantity the total width B of the composite lens feature 16 squared minus the total width T 2 of the circular tip segment 16 a squared, that quantity plus twice the height H 3 of the second elliptical base segment 16 c times the total width T 2 of the circular tip segment 16 a times the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c divided by the tangent contact angle A 51 at the top of the second elliptical base segment 16 c times the quantity the height H 3 of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the quantity of the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a plus quantity the height H 3 of the second elliptical base segment 16 c times the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c the quantities of the divisor times 4.
[0041] The parameter d 5 is equal to the quotient of the quantity twice the height H 3 of the second elliptical base segment 16 c plus the of tangent contact angle A 51 at the top of the second elliptical base segment 16 c times the quantity the total width B of the composite lens feature 16 minus the total width T 2 of the circular tip segment 16 a, the previous quantities times the height H 3 of the second elliptical base segment 16 c divided by the height H 3 of the second elliptical base segment 16 c times 4 plus the quantity plus the tangent of contact angle A 51 at the top of the second elliptical base segment 16 c plus the tangent of contact angle A 52 at the bottom of the second elliptical base segment 16 c times the quantity the total width B of the composite lens feature 16 squared minus the total width T 2 of the circular tip segment 16 a.
[0042] The coordinate x is a value in the direction of the input edge or more specifically in the direction of the total width of the composite lens feature 16 and is preferably set within the range of T 2 /2≦x≦B/2 for the second elliptical base segment 16 c. The coordinate y 5 is a value in the light propagation direction.
[0043] The contact angles for the composite lens feature can be described where A 41 =A 51 , A 42 =A 52 and A 1 ≦A 42 , A 41 . Preferably, A 1 ≦A 42 , A 41 ≦85 degrees.
[0044] FIG. 7 a is a ray tracing for an array of a single composite lens feature 16 of this invention illustrating what happens to the light rays when the individual composite lens features are disposed on the light input surface 12 a in a contiguous manner such that there is no gap G between adjacent composite lenses. FIG. 7 b is a similar ray tracing, but where the individual composite lens feature is separated by a gap G between adjacent features. The gap G is preferably less than or equal to 0.9 P where P (as shown in FIG. 6 b ) is the pitch of the composite lens feature on the input surface 12 a. In FIG. 7 a , where the composite lens features are adjacent each other along the input surface, some of the light rays will experience a secondary light collimation as they are refracted when they reach the side of the adjacent feature. This secondary light collimation detracts from the diffusion capability of the composite lens feature 16 . In FIG. 7 b , the composite lens features are separated by a gap G. The gap allows the light ray to continue in a diffuse manner and thus widens the angle at which the light propagates in the light guide film. There is minimal secondary light collimation when the gap between features is incorporated into the composite lens feature design. In this way, the wider angle of light helps to mitigate the hot spots along the input surface of the light guide film.
[0045] Referring now to FIG. 8 , the light guide film 12 in FIG. 8 shows the composite lens features 16 not disposed along the entire input surface 12 a. Instead, the composite lens features 16 are disposed along the light input surface 12 a in the region where the LED 14 light is incident. The luminance uniformity of the system is minimally affected as the unpatterned region on the light input surface has minimal light rays in this region.
EXAMPLES
[0046] FIG. 9 a shows a portion of the light input surface 32 of a light guide film 30 with an arc- or circular-type structure 36 . The graph in FIG. 9 b illustrates the light intensity for the light guide film 30 at distances 3.5 mm, 4.5 mm and 5.5 mm from the light input surface 32 . FIG. 9 b shows that the localized light intensity decreases as the distance increases from the light input surface, but there are still some hot spots evident at 5.5 mm The arc- or circular-type structure solution provides some improvement for hot spots but is more effective at collimating light in line with the LED than widening the incidence angle. This is evident in the graph in FIG. 9 b . In FIG. 9 b , the LEDs are located at each of the vertical dotted lines and the light distribution is still not leveled out at 5.5 mm into the light guide film. It is apparent from the graph in FIG. 9 b that the arc- or circular-type solution has insufficient diffusion capability.
[0047] FIG. 10 a shows a portion of the light input surface 42 of a light guide film 40 with a composite lens structure that has flat slanted sides 46 . This result would also be applicable to a trapezoidal shaped light input structure. The graph in FIG. 10 b illustrates the light intensity for the light guide film 40 at distances 3.5 mm, 4.5 mm and 5.5 mm from the light input surface 42 . FIG. 10 b shows that the localized light intensity actually inverts in the area immediately in front of the LEDs, resulting in a dark spot immediately in front of the LEDs. This overall loss of light intensity immediately in front of the LED is due to the fact that the straight slanted walls diffuse the light more readily through the sides than through the tip. It is also noted that the shape of the light intensity profile across the light guide film does not change significantly as the distance increases from the input surface 42 .
[0048] FIG. 11 a shows a portion of the light input surface 52 of a light guide film 50 with the composite lens feature 56 of this invention. The composite lens feature utilizes a circular tip segment and two tilted elliptical base segments. The top and bottom contact angles for each of the two tilted elliptical base segments are equal. The top and bottom contact angles for each of the two tilted elliptical base segments are greater than the contact angle of the circular tip segment. The circular tip segment uniformly distributes the light in the area immediately in front of the LED. The two tilted elliptical base segments uniformly distribute the light between the LEDs. The smooth curvatures of the circular tip segment and the two tilted elliptical base segments maximize the uniformity of the light spatial distribution so the output light is uniform. The graph in FIG. 11 b illustrates that the composite lens 56 of the present invention generates uniform light output across the light guide film at distances of 3.5 mm, 4.5 mm and 5.5 mm from the input surface 52 .
[0049] Hence, an improved light guide film is provided with symmetric light redirecting features to improve light output uniformity without sacrificing light input efficiency. Namely, the improved light guide film 12 having composite lens structure 16 provides enhanced light diffusion in the plane parallel to the light extraction plane and light reflection plane (top and bottom surfaces), allowing greater light redistribution between discrete light sources (light traveling outside the critical angle of planar un-serrated input edge), so that the light output uniformity is improved. Moreover, the light distribution in the plane perpendicular to the light extraction plane and light reflection plane (top and bottom surfaces) is minimized, so that the condition of the total internal reflection is minimized for the inputted traveling light. | The present invention provides a planar light guide film for a backlight unit having at least one point light source, the light guide film comprising a light input surface for receiving light from the point light source, a light redirecting surface for redirecting light received from the light input surface and a light output surface for outputting at least the light redirected from the light redirecting surface. The light input surface further comprises a composite lens structure having a circular tip segment with a first contact angle, and a first and second elliptical base segments with a second contact angle, the second contact angle being greater than the first contact angle and the second contact angle being equal to each other and
wherein the circular tip segment satisfies the following equation:
y 1 =a 1 +√{square root over (( r 1 2 −x 2 ))}
and the elliptical base segments satisfies the following equations:
y 4 =d 4 +b 4 ×√{square root over ((1−(( x+c 4 )/ a 4 ) 2 )}
y 5 =d 5 +b 5 ×√{square root over ((1−(( x−c 5 )/ a 5 ) 2 )} | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not applicable
INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC
[0003] Not applicable
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] This invention relates generally to removable storm and hurricane shutters, and more particularly to an end cap dependently engagable within each end of an upper H-header for supporting the corners of a corrugated hurricane shutter.
[0006] 2. Description of Related Art
[0007] Hurricane shutters have become extremely popular and useful in the hurricane prone sections of the country. Such hurricane shutters are typically deployed prior to an area coming under the influence tropical storm and hurricane weather conditions and serve to prevent damage to the glass windows and portal doors as a result of high winds and flying debris.
[0008] An example of such a storm shutter installation is disclosed in U.S. Pat. No. 4,685,261. This invention is primarily directed to a hurricane shutter which includes a lower support channel or bracket which is readily adaptable to a range of lower sill angles to which this portion of the storm shutter is attached.
[0009] A critical aspect with respect to this type of hurricane shutter, and with all hurricane shutters, is that it must meet stringent impact testing requirements before becoming approved for use as a hurricane damage preventative. One such test such hurricane shutters must pass is to withstand substantial deformity and damage from heavy object high speed impact. It has been shown that, although the polycarbonate corrugated hurricane shutter structure is generally adequate to withstand such impact, when incorporated into conventional H-headers for support, impact in the vicinity of the upper portions of the hurricane shutter results in excessive deformation of the corrugations and expansion of those corrugations, causing the structure to fail building code testing.
[0010] The present invention affords a simple end cap structure which is positionable within each end of an upper H-header for strengthening and stabilizing the shape of the upper corners of a corrugated polycarbonate hurricane shutter to eliminate excessive corrugation deformation in the upper corner areas and lateral expansion movement of the hurricane shutter which otherwise results in failure to comply with current building code testing procedure.
[0011] The foregoing examples of the related art and limitations related therewith are intended to be illustrative and not exclusive. Other limitations of the related art will become apparent to those skilled in the art upon a reading of the specification and a study of the drawings.
BRIEF SUMMARY OF THE INVENTION
[0012] This invention is directed to an end cap for an H-shaped header bar used to secure a corrugated polycarbonate hurricane shutter attachable to a window frame. The H-header has a generally inverted U-shaped pocket adapted in size to receive an upper margin of the hurricane shutter, with the end cap positioned in each end of the header bar. The H-header cooperates with a lower support channel also attached to the window frame to support and secure the hurricane shutter over the window. The end cap is dependently positionable within an inner upright side of the pocket to engage with the upper corner of the hurricane shutter, strengthening and preventing substantial movement from flying object impact during heavy hurricane wind conditions and building code testing therefor.
[0013] It is therefore an object of this invention to provide an end cap securable around each upper corner of a polycarbonate corrugated hurricane shutter and dependently positionable within the ends of the header to strengthen and prevent unacceptable upper corner deformation and expansion movement of the hurricane shutter during hurricane and tropical storm conditions.
[0014] It is therefore an object of this invention to provide an end cap securable around each upper corner of a polycarbonate corrugated hurricane shutter and dependently positionable within the ends of the header to strengthen and prevent unacceptable upper corner deformation and expansion movement of the hurricane shutter during hurricane and tropical storm conditions during building code testing procedures.
[0015] The following embodiments and aspects thereof are described and illustrated in conjunction with systems, tools and methods which are meant to be exemplary and illustrative and not limiting in scope. In various embodiments one or more of the above-described problems have been reduced or eliminated while other embodiments are directed to other improvements. In addition to the exemplary aspects and embodiments described above, further aspects and embodiments will become apparent by reference to the drawings and by study of the following descriptions.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
[0016] FIG. 1 is a perspective exploded view of the present invention incorporated into each end of an H-header and supporting the upper corner of a corrugated hurricane shutter.
[0017] FIG. 2 is a simplified exploded top plan view of the upper right-hand corner of FIG. 1 showing the H-header in phantom.
[0018] FIG. 3 is an exploded top plan view similar to FIG. 2 showing another embodiment of the invention.
[0019] FIG. 4 is a perspective view of a third embodiment of the invention.
[0020] FIG. 5 is an end elevation view of FIG. 4 .
[0021] FIG. 6 is a rear elevation view of FIG. 4 .
[0022] FIG. 7 is a front elevation view of FIG. 5 .
[0023] FIG. 8 is a perspective view of a fourth embodiment of the invention.
[0024] FIG. 9 is an end elevation view of FIG. 8 .
[0025] FIG. 10 is a front elevation view of FIG. 8 .
[0026] FIG. 11 is another end elevation view of FIG. 8 .
[0027] FIG. 12 is a side elevation view of FIG. 8 .
[0028] FIGS. 8A and 12A show an alternate embodiment to that shown in FIGS. 8 and 12 .
[0029] FIG. 13 is a perspective view of a fifth embodiment of the invention.
[0030] FIG. 14 is a top plan view of FIG. 13 .
[0031] FIG. 15 is a front elevation view of FIG. 14 .
[0032] FIG. 16 is a bottom plan view of FIG. 14 .
[0033] Exemplary embodiments are illustrated in reference figures of the drawings. It is intended that the embodiments and figures disclosed herein are to be considered to be illustrative rather than limiting.
DETAILED DESCRIPTION OF THE INVENTION
[0034] Referring now to the drawings, and firstly to FIG. 1 , a typical hurricane shutter is there shown generally at numeral A which includes a corrugated polycarbonate transparent hurricane shutter D supported along a lower horizontal margin thereof by an upright U-shaped lower channel E and, along an upper margin of the hurricane shutter D within an inverted downwardly extending H-header B.
[0035] Referring additionally to FIG. 2 , absent the present invention which is shown generally at numeral 10 , the corrugations F of the hurricane shutter D simply sit within the upright side walls of the header B and are somewhat free to move laterally as well as front to back absent substantial support. However, the present invention 10 is positionable within the ends of the header B and fitted downwardly and entrappingly around the upper corner of each of the edge corrugations J. Note that the end cap 10 is not shown at the lower end of the header B for simplicity, but may be added.
[0036] The end cap 10 is formed of either extruded or roll-formed thin wall plastic or sheet metal material, and preferably polycarbonate for strength having an overall width that slidably engages into the header B shown in phantom in FIG. 2 . The end cap 10 includes a housing 12 having a flat front wall 24 extending into an arcuate inner side wall 14 and an outer side wall 22 having an offset at 18 forming a stop, the purpose of which is described herebelow. The housing 12 also includes an upright back wall 20 which, in combination with the end of the arcuate side wall 12 , forms an upright access slot 16 extending over the entire height of the housing 12 .
[0037] The above housing configuration is sized and adapted to downwardly slide over the corner of the edge corrugation J as shown. The access slot 16 is slidable downwardly over the second arcuate portion K of corrugation J, the first flat corrugation J bearing against the inner surface of the back wall 20 , while the first arcuate portion L terminating at edge C, bears against the end stop 18 . The small gap 26 between the neutral portion N of the first corrugation provides very limited clearance or no clearance at all with a biased engagement against the arcuate portion 14 so as to establish a non-movable non-deforming arrangement laterally, while the front wall 24 and the rear wall 20 bearing against the corresponding upright sides of the H-header B prevent any fore and aft (or front-to-back) movement, thus fully entrapping the upper corner of the hurricane shutter D. Appropriate fasteners (not shown) may further interengage these mating upright front and back surfaces with the side walls of the H-header B as desired.
[0038] Referring now to FIG. 3 , a second embodiment of the invention is there shown wherein the front upright surface 44 extends across a more substantial length of the housing 32 while still maintaining an end stop 38 for supportingly bearing against the upright edge C of the hurricane shutter D. As previously described, the flat M of the first corrugation J bears against the rear upright wall 40 while the first neutral portion N is closely spaced at 46 with respect to the arcuate inner side wall 34 . The outer side wall 42 , in combination with stop surface 38 , entraps the edge C of the hurricane shutter D.
[0039] Referring now to FIGS. 4 to 7 , a third embodiment of the invention is there shown generally at numeral 50 and also includes a molded or extruded plastic or metal housing 52 having an arcuate inner side wall 54 which in combination with the upright back panel 60 forms the access slot 56 which functions as previously described. The combination of the stop surface 58 and the outer side wall 62 define an entrapment means similar to that previously described. The front upright surface 64 is again elongated similar to that shown in FIG. 3 .
[0040] Referring now to FIGS. 8 to 12 , a fourth embodiment of the invention is there shown generally at numeral 70 and also includes a molded plastic or metal housing 72 having an inner arcuate surface 74 blending uniformly from the front upright surface 84 . The back upright surface 80 defines, in combination with the end of the inner side wall 74 , the access slot 76 . The front upright wall 84 is of a length similar to that in FIG. 3 , while the combination of outer upright side wall 82 and stop surface 78 define the entrapment means for the edge C of the upper corner of the hurricane shutter D as previously described. In this embodiment of the housing 72 , a solid top surface 86 is also provided as an end stop for the upper end corner of the first corrugation J of the hurricane shutter D for added stability.
[0041] FIGS. 8A and 12A show an alternate embodiment of the invention shown at numeral 70 in FIGS. 8 and 12 . This embodiment 70 ′ includes all of the features previously described in FIGS. 8 and 12 with respect to embodiment 70 , except for the addition of a lead-in ramp 88 which extends diagonally into panel 88 a . This enlarges the size and breadth of the slot 76 ′ defined from the inner arcuate surface 74 ′. This lead-in ramp 88 and enlarged access slot 76 ′ greatly facilitate the assembly of this embodiment 70 ′ over the upper corner of the corrugated panel D.
[0042] Referring lastly to FIGS. 13 to 16 , a fifth embodiment is there shown at numeral 90 having a molded plastic or metal thin wall housing 92 similar to that previously described. The front upright surface 104 blends into the convex arcuate inner side wall surface 94 and, in combination with the upright back wall 100 , defines the corrugation access slot 96 for the upper corner of the corrugated hurricane shutter D as previously described.
[0043] In this embodiment 90 , the housing 92 includes a reinforcing gusset 108 which does not interfere with the entrapment functioning of the outer end wall 102 in combination with the stop surface 98 . A panel 106 is positioned centrally along the height of this embodiment 92 which bears against the upper end of either of the corners of the corrugated hurricane shutter D so as to achieve ambidextrous structure, that is, this embodiment 90 will fit on either upper end of the corners of the hurricane shutter D.
[0044] All of the above described embodiments provide two important strengthening and building code qualifying aspects necessary for these polycarbonate corrugated hurricane shutters to both meet building code requirements and to adequately protect the contents and people within a so-protected building window structure. The first aspect is with respect to the deformation of the corner areas of the corrugated storm shutter which otherwise occurs causing test failure when struck by a high impact flying object. Additionally, when the corrugated hurricane shutter is struck in a central upper portion, the collapse of the corrugations in the impact area has been shown to otherwise lead to the lateral expansion of the structure in the vicinity of the upper corners causing test failure as well. The present invention both restrains the upper corners from corrugation deformation and restrains the overall corrugation structure from excessive lateral expansion by semi-rigidly restraining these corner areas from such outward lateral movement.
[0045] While a number of exemplary aspects and embodiments have been discussed above, those of skill in the art will recognize certain modifications, permeations and additions and subcombinations thereof. It is therefore intended that the following appended claims and claims hereinafter introduced are interpreted to include all such modifications, permeations, additions and subcombinations that are within their true spirit and scope. | An end cap for an H-shaped header bar used to secure a corrugated hurricane shutter attachable to a window frame and having a generally inverted U-shaped pocket adapted in size to receive an upper margin of the hurricane shutter and the end cap at each end of the header bar. The header bar cooperates with a lower support channel also attached to the window frame to support and secure the hurricane shutter over the window. An end cap is positionable and attachable within an inner upright side of the pocket to engage with the upper corner of the hurricane shutter preventing substantial lateral expansion movement or corrugation deformation from being struck by flying objects during heavy hurricane wind. | 4 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/619,840, filed on Oct. 18, 2004.
FIELD OF THE INVENTION
[0002] The present invention relates to hose couplings, and more particularly to hose couplings including a plastic ferrule which militates against a hose end being released from the hose coupling during use.
BACKGROUND OF THE INVENTION
[0003] A traditional stamped coupling set consists of a male element or a female element and a ribbed ferrule. All of the elements are typically made of brass. A ribbed ferrule is placed over the outside circumference of a hose, and a tailpiece of the male/female element is inserted into the interior of the hose. A set of expandable fingers is inserted into the tailpiece and then activated, causing the fingers to expand and push the tailpiece outwardly, thereby pinching the hose between the tailpiece and the ribbed ferrule. Traditional couplings utilize fingers which shape the tailpiece in a wave or wrinkled form.
[0004] When the coupling having the tailpiece in the wave form is subject to a pull test, the hose quickly loses contact with the tailpiece and the associated ribbed ferrule. When the hose elongation reaches the next corresponding rib of the ferrule, almost no surface area of the hose is sustained up to the next adjacent compressed area.
[0005] It is considered to be advantageous if the present coupling structures could be designed to increase the overall strength and simultaneously reduce the cost to manufacture the product.
[0006] It would be desirable to produce a garden hose coupling assembly which is of improved strength and is less expensively manufactured.
SUMMARY OF THE INVENTION
[0007] In accordance with the current invention, a hose coupling wherein a strength thereof is maximized and a cost of manufacture is minimized has been surprisingly discovered.
[0008] The invention is typically produced by changing the composition and geometry of a ferrule which is used together with a tailpiece of a male or female coupling to compressively retain a section of a hose.
[0009] It is one purpose of the invention to embrace a new composition and geometry of the ferrule in order to maintain constant contact between the elements of the coupling and the associated hose. A ferrule in accordance with the current invention maintains a substantially constant inner diameter and acts as a boundary toward which the tailpiece is expanded. Once the expansion of the tailpiece is accomplished, the hose is tightly held in a compressed state between the outer surface of the expanded portion of the tailpiece and the inner surface of the surrounding ferrule.
[0010] It is another purpose of the invention to utilize a ferrule made of plastic to reduce the cost of manufacturing.
[0011] In one embodiment, the hose coupling comprises: a hollow cylindrical coupling having a first end and a second end, a threaded section formed adjacent the first end, and a tailpiece formed at the second end adapted to be received in an end of a hose; and a hollow plastic ferrule having a radially inwardly extending lip formed at a first end thereof, the ferrule surrounding at least a portion of the tailpiece of the coupling and cooperating with the tailpiece to secure the end of the hose therebetween.
[0012] In another embodiment, the hose coupling comprises: a hollow cylindrical coupling having a first end and a second end, the first end including a threaded section for receiving a complimentary threaded section of an associated coupling, the second end including a tailpiece adapted to be received in an end of a hose, the coupling including a shoulder formed between the first end and the second end, and an annular groove formed between the shoulder and the second end of the coupling; and a hollow plastic ferrule having a first end and a second end, the first end having a radially inwardly extending lip which abuts the shoulder of the coupling, an inner surface of the ferrule having a substantially constant diameter, the ferrule surrounding at least a portion of the tailpiece of the coupling and cooperating with the tailpiece to secure the end of the hose therebetween.
[0013] The invention also provides methods of forming hose couplings. In one embodiment, the method of forming the hose coupling comprises the steps of: providing a hollow cylindrical coupling having a first and a second end, a threaded section formed adjacent the first end for receiving a complimentary threaded section of an associated coupling, a tailpiece formed at the second end; causing the interior of a hose to be disposed around at least a portion of the tailpiece of the coupling; providing a hollow plastic ferrule having a first end and a second end, the first end of said ferrule terminating in radially inwardly extending lip; causing the hollow plastic ferrule to be disposed around the tailpiece and the hose; and causing the tailpiece of the coupling and to expand outwardly to secure the hose between the tailpiece and the ferrule.
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The above, as well as other advantages of the present invention, will become readily apparent to those skilled in the art from reading the following detailed description of several embodiments of the invention when considered in the light of the accompanying drawings, in which:
[0015] FIG. 1 is a sectional side view of a hose coupling according to an embodiment of the invention;
[0016] FIG. 2 is a side view partially in section of a hose coupling similar to the coupling illustrated in FIG. 1 including a female coupling;
[0017] FIG. 3 is a side sectional view of a hose coupling according to another embodiment of the invention;
[0018] FIG. 4 is a side view partially in section of a hose coupling similar to the coupling illustrated in FIG. 3 including a female coupling.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0019] The following detailed description and appended drawings describe and illustrate various exemplary embodiments of the invention. The description and drawings serve to enable one skilled in the art to make and use the invention, and are not intended to limit the scope of the invention in any manner. In respect of the methods disclosed and illustrated, the steps presented are exemplary in nature, and thus, the order of the steps is not necessary or critical.
[0020] FIG. 1 illustrates a hose coupling 10 consisting of a male coupling 12 and an associated hollow ferrule 14 . The male coupling 12 is typically formed of metal, such as brass for example. The male coupling 12 includes a male threaded section 16 formed adjacent a first end thereof for receiving a complimentary threaded section of an associated female coupling (not shown). A tailpiece 18 is formed at a second end of the male coupling 12 and includes a plurality of ribs 20 formed thereon. It is understood that the number of ribs 20 is not regarded as critical. A shoulder 22 is formed between the threaded section 16 and the tailpiece 18 . An inwardly extending annular groove 23 is disposed between the shoulder 22 and the tailpiece 18 .
[0021] The hollow ferrule 14 is positioned to surround the end of an associated hose 30 . The ferrule 14 may be formed of a plastic material, such as nylon, for example. A radially inwardly extending lip 24 is formed at a first end of the hollow ferrule 14 . An inner surface 26 of the hollow ferrule 14 includes a plurality of grooves 28 formed thereon. It is understood that more or fewer grooves than shown can be used as desired.
[0022] The end of the hose 30 is disposed radially between the tailpiece 18 and the hollow ferrule 14 . The hose 30 is typically inserted a garden hose, for example. Additionally, the hose 30 can be formed of any conventional material such as rubber, for example.
[0023] A method of forming the hose coupling 10 according to the embodiment of the invention shown in FIG. 1 will now be described. The male coupling 12 is provided. The end of the hose 30 is disposed around the tailpiece 18 . The hollow ferrule 14 is disposed around the hose 30 and positioned as shown in FIG. 1 . The radially inwardly extending lip 24 of the hollow ferrule 14 is caused to abut the shoulder 22 of the male coupling 12 .
[0024] A tool having a set of expandable fingers (not shown) is inserted into the male coupling 12 and activated. The fingers are cause to expand, thereby causing the tailpiece 18 of the male coupling 12 to expand outwardly toward the hollow ferrule 14 to form the ribs 20 and the annular groove 23 . The hose 30 is secured between the tailpiece 18 and the hollow ferrule 14 . The lip 24 and the groove 23 cooperate to militate against relative movement between the male coupling 12 and the ferrule 14 . It is understood that alternate means of causing the tailpiece 18 to expand and secure the hose 30 can be utilized without departing form the scope of the invention. When the forming tool is removed from the male coupling 12 , the hose coupling 10 is assembled on the associated hose 30 and is ready for use.
[0025] FIG. 2 illustrates a hose coupling 32 including a female coupling 34 . Structure similar to that illustrated in FIG. 1 includes the same reference numeral and a prime (′) symbol for clarity. The female coupling 34 includes a female threaded section 36 for receiving a complimentary threaded section of an associated male coupling (not shown). A method of forming the hose coupling 32 is the same as described for FIG. 1 .
[0026] FIG. 3 illustrates a hose coupling 38 according to another embodiment of the invention. Structure similar to that illustrated in FIGS. 1 and 2 includes the same reference numeral and a double prime (″) symbol for clarity. The hose coupling 38 includes a male coupling 12 ″ and an associated hollow ferrule 40 . The male coupling 12 ″ is typically formed of metal such as brass, for example. The male coupling 12 ″ includes a threaded section 16 ″ formed adjacent a first end thereof for receiving a cooperating with an associated internally threaded section of an associated female coupling (not shown). A tailpiece 18 ″ is formed at a second end of the male coupling 12 ″. A shoulder 22 ″ is formed between the threaded section 16 ″ and the tailpiece 18 ″. An annular groove 23 ″ is disposed between the shoulder 22 ″ and the tailpiece 18 ″.
[0027] The hollow ferrule 40 may be formed of a plastic material such as nylon, for example. A radially inwardly extending lip 24 ″ is formed at a first end of the hollow ferrule 40 . An inner surface 42 of the hollow ferrule 40 is smooth and uninterrupted and has a substantially constant inner diameter from the radially inwardly extending lip 24 ″ to an opposing edge portion 44 thereof.
[0028] The method of forming the hose coupling 38 will now be described. The male coupling 12 ″ is provided. The end of the hose 30 ″ is disposed around the tailpiece 18 ″ of the coupling 12 ″. The hollow ferrule 40 is disposed around a hose 30 ″ and is positioned as shown in FIG. 3 . The radially inwardly extending lip 24 ″ of the hollow ferrule 40 is caused to abut against the shoulder 22 ″ of the male coupling 12 ″.
[0029] A tool having a set of expandable fingers (not shown) is inserted into the male coupling 12 ″ and activated. The fingers are caused to expand, thereby causing the tailpiece 18 ″ of the male coupling 12 ″ to expand outwardly toward the hollow ferrule 40 . The hose 30 ″ is thereby secured between the tailpiece 18 ″ and the hollow ferrule 40 . The lip 24 ″ and the groove 23 ″ cooperate to militate against relative movement between the male coupling 12 ″ and the ferrule 40 . It is understood that alternate means of causing the tailpiece 18 ″ to expand and secure the hose 30 ″ can be utilized without departing form the scope of the invention.
[0030] FIG. 4 illustrates a hose coupling 46 including a female coupling 34 ′″. Structure similar to that illustrated in FIGS. 1 , 2 , and 3 includes the same reference numeral and a triple prime (′″) symbol for clarity. The female coupling 34 ′″includes an internally threaded section 36 ′″ for receiving a complimentary threaded section of an associated male coupling (not shown). The method of forming the hose coupling 46 is the same as described for FIG. 3 .
[0031] The use of a plastic ferrule provides several advantages over the prior art, including a lower cost of manufacturing than the traditional structure typically utilizes a brass ferrule. In addition to the cost savings, the use of a plastic ferrule allows for variations in color and the addition of trademarks and other indicia on the plastic ferrule which would be attractive in the marketplace.
[0032] From the foregoing description, one ordinarily skilled in the art can easily ascertain the essential characteristics of the invention and, without departing from the spirit and scope thereof, can make various changes and modifications to adapt it to various usages and conditions. | A hose coupling and method of forming the same are disclosed, wherein a strength thereof is maximized and a cost of manufacture is minimized. The hose coupling utilizes a plastic ferrule which militates against a hose end being released from the hose coupling during use. | 5 |
This is a division of patent application Ser. No. 08/901,646, filing date Jul. 28, 1997, now U.S. Pat. No. 5,843,816.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to MOSFET semiconductor memory integrated circuits devices and more particularly to improved full Complementary Metal Oxide Semiconductor (CMOS) Static random access memory (SRAM) memory cells.
2. Description of Related Art
Integrated circuit (IC) memory devices are made up of a plurality of memory cells. In general, one basic memory cell design is duplicated numerous times to form those cells. The basic cell design may be modified slightly from cell to cell, for example one cell may be a reversed image or complement of an adjacent cell, but the entire memory device can be described according to the basic cell design.
In the case of Static Random Access Memory (SRAM) devices, the basic cell is usually in one of two forms, either a six transistor (6T) cell or four transistor/two resistor (4T/2R) cell. Many conventional SRAMs using a 6T configuration have six transistors formed in a bulk semiconductor substrate such as single crystal silicon. That type of SRAM is usually embodied in a Complementary Metal Oxide Semiconductor (CMOS) technology, with four transistors being N-channel devices while the remaining two transistors are P-channel devices. A 6T SRAM device operates at relatively low power levels and the bulk transistors have good electrical characteristics, including high mobility and low threshold voltages. Also 6T SRAMs are relatively stable, having high immunity to cell errors, such as those caused by incident alpha particles. However, 6T SRAM cells formed of transistors in a bulk substrate require a large area because the transistors are formed next to one another in the substrate and are essentially in the same plane; which use of six bulk transistors imposes an undesirable lower limit on the cell size. Achieving the smallest cell size with the simplest process reduces the manufacturing costs, increases memory capacity, and increases the device performance without increasing the overall device size.
U.S. Pat. No. 5,394,358 of Huang for "SRAM Memory Cell with Tri-level Local Interconnect" shows a method of forming a 6T SRAM that reduces the number of local interconnections. However, these patents do not show the butted contact structure of the invention.
U.S. Pat. No. 5,330,929 of Pfiester et al. for "Method of Making a Six Transistor Static Random Access Memory Cell" shows a method of making a six transistor (6T) SRAM Cell. However, Pfiester et al. does not show the butted contact of this invention, but does include an SRAM cell and a method of forming a memory cell, wherein the memory cell may comprise an active region and a first layer. The active region include first, second and third segments. The first segment has an adjacent end and a distal end. The second segment, generally parallel to the first segment, has an adjacent end and a distal end. For the third segment, generally perpendicular to the first direction, the adjacent end of the first segment lies near an end of the third segment. The adjacent end of the second segment lies near the other end of the third segment. The first layer is shaped similarly to the active region except that the first layer does not lie over the first and second segments near the distal ends. This invention includes an SRAM cell and a method of forming the memory cell, wherein the memory cell comprises shared gate gate electrodes that overlap one another without electrically contacting each other.
DEFINITIONS
Self-Aligned Source/Drain Regions:
Regions formed in a silicon crystal substrate by ion implanting using the gate electrode itself as a mask to align the source/drain regions to the gate electrode.
Self-Aligned Contact:
A contact formed to a region of the substrate which is self-aligned with the polysilicon conductor structure of an MOS device.
Butted contact:
In a silicon gate MOS device, a polysilicon conductor and the active device region "butt" up against each other but do not make direct electrical contact with each other. There is an indirect form of electrical contact between the polysilicon conductor layer and the substrate wherein the polysilicon conductor is aligned with the edge of the active-device region to which contact is to be made. A contact window is opened that overlaps the polysilicon conductor and the active device region of the substrate. Metal is deposited into the window to form an electrical contact between the conductor and the active device region.
SUMMARY OF THE INVENTION
In accordance with this invention, a method if provided for forming a contact between a conductor and a substrate region in a MOSFET device is made by the following steps. Form a semiconductor substrate with a silicon oxide layer formed on the surface thereof. Form a stack of a conductor material upon the surface of the silicon oxide layer and form a first dielectric layer upon the conductor material. Pattern the conductor stack into conductors. Form a butted contact pattern in the first dielectric layer by removal of the dielectric layer in at least one butted contact region. Form doped regions in the substrate self-aligned with the conductors. Form a second dielectric layer over the device and patterning the second dielectric layer with contact openings therethrough down to the substrate and to the butted contact region. Form contacts to the substrate and the butted contact regions on the conductor through the contact openings.
Preferably the method includes these steps. Form an etch stop layer over the device before forming the second dielectric layer; employ the etch stop layer when patterning the second dielectric layer; and remove exposed portions of the etch stop layer subsequent to patterning the second dielectric layer.
Preferably, form the first dielectric layer as a silicon dioxide cap.
Preferably, form a barrier layer in the contact openings prior to forming the contacts, and form the contacts on the surfaces of the barrier layer.
Preferably, form lightly doped regions in the substrate and then form spacer structures adjacent to the conductors prior to forming the doped regions in the substrate.
In accordance with another aspect of this invention a contact between a conductor and a substrate region in a MOSFET device is formed by the following steps. Form a semiconductor substrate with a silicon oxide layer formed on the surface thereof and Shallow Trench Isolation (STI) regions in the surface of the substrate. Form a stack of a conductor material upon the surface of the silicon oxide layer and form a first dielectric layer upon the conductor material. Pattern the conductor stack into conductors with at least one thereof juxtaposed with a first STI region. Form a butted contact pattern in the first dielectric layer by removal of the dielectric layer in at least one butted contact region juxtaposed with an STI region. Form doped regions in the substrate self-aligned with the conductors with at least one butted with a the conductor to form a butted contact region. Form a second dielectric layer over the device and patterning the second dielectric layer with contact openings therethrough down to the substrate and to the butted contact region. Form contacts to the substrate and the butted contact regions on the conductor through the contact openings.
Preferably form an etch stop layer over the device before forming the second dielectric layer; employ the etch stop layer when patterning the second dielectric layer; and remove exposed portions of the etch stop layer subsequent to patterning the second dielectric layer.
Preferably, the first dielectric layer is a silicon dioxide cap.
Preferably, form a barrier layer in the contact openings prior to forming the contacts, and form the contacts on the surfaces of the barrier layer.
Preferably, form lightly doped regions in the substrate and then forming spacer structures adjacent to the conductors prior to forming the doped regions in the substrate.
Preferably, form the first dielectric layer as a silicon dioxide cap; form an etch stop layer over the device prior to forming the second dielectric layer, employ the etch stop layer when patterning the second dielectric layer; and remove exposed portions of the etch stop layer subsequent to patterning the second dielectric layer.
Preferably, form a barrier layer in the contact openings prior to forming the contacts, and forming the contacts on the surfaces of the barrier layer.
In accordance with still another aspect of this invention a MOSFET device with a contact between a conductor and a substrate region in the device includes the following features. A semiconductor substrate with a silicon oxide layer formed on the surface thereof has a stack of a conductor material formed upon the surface of the silicon oxide layer with a first dielectric layer upon the conductor material. The conductor stack is formed into conductors. A butted contact pattern is formed in the first dielectric layer with an absence of the dielectric layer in at least one butted contact region. There are doped regions formed in the substrate self-aligned with the conductors. A second dielectric layer is formed over the device patterned with contact openings therethrough down to the substrate and to the butted contact region. There are contacts to the substrate and the butted contact regions on the conductor formed through the contact openings.
Preferably, an etch stop layer is formed over the second dielectric layer except where the contacts are formed.
Preferably, the first dielectric layer is a silicon dioxide cap.
Preferably, there is a barrier layer in the contact openings forming a base for the contacts.
BRIEF DESCRIPTION OF THE DRAWINGS
The foregoing and other aspects and advantages of this invention are explained and described below with reference to the accompanying drawings, in which:
FIG. 1 shows a circuit diagram of a six transistor (6T) Static Random Access Memory (SRAM) cell 10 which includes a first storage node N1 and a second storage node N2 in accordance with this invention.
FIGS. 2A-2I, which are sections taken along line 2-2' in FIG. 4, illustrate a sequence of steps in accordance with the method of formation of a device in accordance with this invention.
FIGS. 3A-3I which are sections taken along line 3-3' in FIG. 4 also illustrate the sequence of steps in accordance with the method of formation of a device in accordance with this invention.
FIG. 4 is a plan view of a device in accordance with this invention.
FIGS. 5A and 5B show a flow chart for the method of manufacture of a device in accordance with this invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
For maximum density to be achieved in a six transistors Static Random Access Memory (6T SRAM) device, the cells must be laid out to have minimum size, i.e occupy as small an area as possible. But conventional device layouts make it difficult to shrink device size due to metal routing and the number of contacts. In accordance with the Self-Aligned BuTt Contact (SABTC) design and method of the present invention, that problem is overcome.
Achieving MOSFET's with low series resistance, in the S/D diffusion layer, in a 6T SRAM device represents a key issue which must be accomplished to realize high-performance CMOS devices. The use of a silicon nitride etch stop layer combined with a modified Self-Aligned Contact (SAC) process to form contacts including butted contacts, provides minimum resistance in the Source/Drain (S/D) regions while at the same time permitting achievement of higher packing densities in accordance with this invention.
FIG. 1 shows a circuit diagram of a six transistor (6T) Static Random Access Memory (SRAM) cell 10 which includes a first storage node N1 and a second storage node N2 in accordance with this invention. A first pass transistor T3, a first latch transistor T1 and a first load transistor T5 are associated with the first storage node N1. A second pass transistor T4, a second latch transistor T2 and a second load transistor T6 are associated with the second storage node N2.
The gate electrodes for the first latch transistor T1 and the first load transistor T5 are connected via conductor line 16 to the second storage node N2. The gate electrodes for the second latch transistor T2 and the second load transistor T6 are connected via conductor line 26 to the first storage node N1. The gate electrodes for the pass transistors T3 and T4 are connected via lines 14 and 24, respectively, to the word line WL.
The source regions of load transistors T5 and T6 are electrically interconnected, as well as being connected to a V cc terminal via Self-Aligned Contacts SAC1 (via line 18) and SAC2 (via line 28) respectively.
The source regions of the latch transistors T1 and T2 are electrically interconnected, as well as being connected to a V ss terminal and connected together via Self-Aligned Contacts SAC3 (via line 19) and SAC4 (via line 29). The V ss terminal is at reference potential, when in operation.
The source/drain circuit of the pass transistor T3 is connected via Self-Aligned Contacts SAC5 and SAC6, respectively between the bit line BL bar (line 12) and node N1.
The source/drain circuit of the pass transistor T4 is connected via Self-Aligned Contacts SAC7 and SAC8, respectively between the node N2 and the bit line BL (line 22).
The pass and latch transistors T1, T2, T3, T4 are NMOS (N-channel) devices and the load transistors are PMOS (P-channel) T5, T6 devices.
There is a Self-Aligned BuTt Contact (SABTC) BC1 connected to the Node N2 and the conductor line 16 which interconnects the gate electrodes of the first latch transistor T1 and the first load transistor T5.
There is also a Self-Aligned BuTt Contact (SABTC) BC2 connected to the Node N1 and the conductor line 26 which interconnects to the gate electrodes of the first latch transistor T2 and the first load transistor T6.
On the one hand interconnection line I1 interconnects node N2 to Self-Aligned BuTt Contact (SABTC) BC1 and the conductor line 16. On the other hand, interconnection line I2 connects node N1 to Self-Aligned BuTt Contact (SABTC) BC2 and the conductor line 26.
Method of Forming Self-Aligned BuTt Contact (SABTC)
The method of forming a device in accordance with the plan view seen in FIG. 4 as illustrated in FIGS. 2A-2I which are sections taken along line 2-2' in FIG. 4 and as illustrated in FIGS. 3A-3I which are sections taken along line 3-3' in FIG. 4 which is a plan view of a device in accordance with this invention.
Referring to FIGS. 2A and 3A, after performance of early steps preparatory to performance of the process of this invention is illustrated. Referring to the flow chart in FIGS. 5A and 5B, in step 50 in FIG. 5A, active regions AR in FIG. 4 are formed in a P- substrate 31 of device 30, as will be understood by those skilled in the art.
Next, in step 52 in FIG. 5A, a Shallow Trench Isolation (STI) process has been performed to form STI trenches in the substrate 31. The trenches are filled with silicon dioxide STI region 33A in FIG. 2A and STI regions 33B and 33C in FIG. 3A, in accordance with STI process steps well known to those skilled in the art. Alternatively a LOCOS (LOCal Oxidation of Silicon) process can be used. Relative to STI and LOCOS processes, see Wolf, "Silicon Processing for the VLSI Era Vol. 3--The Submicron MOSFET", Pages 330-420.
In the process a gate oxide layer 32 is formed during the STI or LOCOS process on the remaining surface of the substrate 31, as is usual.
Next, in step 54 of FIG. 5A, as shown in FIGS. 2A and 3A, a blanket of gate conductor electrode layer G1/G2/G3/G4 was deposited over the silicon dioxide STI/LOCOS structures 33A, 33B, 33C and gate oxide layer 32. The gate conductor material comprises ether doped polysilicon or doped polycide/doped polysilicon with a thickness from about 1500 Å to about 3500 Å.
Referring again to FIGS. 2A and 3A, in step 56 a hard mask has been formed as a silicon dioxide cap layer OX1/OX2/OX3/OX4 deposited over the blanket gate conductor electrode layer G1/G2/G3/G4. The silicon dioxide cap (hard mask) layer OX1/OX2/OX3/OX4 is formed by a conventional CVD (Chemical Vapor Deposition) TEOS (Tetra-Ethyl-Ortho Silicate) process which is selected from Plasma Enhanced CVD TEOS (PECVD TEOS) or Low Pressure CVD TEOS (LPCVD TEOS) process with a thickness from about 1,000 Å to about 2,500 Å.
In step 58 a gate conductor mask has been formed over the gate conductor electrode layer and the silicon dioxide cap. Then etching through the mask has formed the four gate electrode stacks G1/OX1, G2/OX2, G3/OX3, and G4/OX4 as seen in FIG. 2A.
In step 60, in FIG. 5A as shown in FIG. 2A, the Lightly Doped Drain & source (LDD) process was performed with N-LDD regions formed in a P-Substrate as shown in FIG. 2A or the alternative of P-LDD regions in the N-Substrate, not shown herein. The NLDD P31 or As dopant is applied in a range from about 1E13 ions/cm -2 to about 1E14 ions/cm -2 at an energy from about 20 keV to about 50 keV. The PLDD BF 2 dopant is applied in a range from about 1E13 ions/cm -2 to about 1E14 ions/cm -2 at an energy from about 20 keV to about 50 keV.
In step 62 (FIG. 2B) a Butt Contact (BC) mask PR1 with an opening W1 is formed over the device of FIG. 2A.
In step 64 of FIG. 5A (FIG. 2C) the Butt Contact (BC) region (of the device of FIG. 2B) has been patterned by etching away the left portion of the silicon dioxide cap OX2 exposed through the opening W1 in mask PR1, leaving the upper surface of gate electrode G2 exposed. In the case of FIG. 3C, the cap OX2 is shown etched away on the right, and there is a trough 37 etched down into the STI region 33C to the right of gate electrode G2. Then the mask PR1 is stripped away from the device 30 leaving the four gate electrode stacks G1/OX1, G2/OX2, G3/OX3, and G4/OX4 exposed.
In step 66, in FIG. 5A as shown in FIGS. 2D and 3D, the device of FIG. 2C is shown after silicon dioxide spacers 38 have been formed in accordance with the well known spacer formation process steps of deposition of silicon dioxide and etching back the silicon dioxide layer with a dry etching (RIE) process. Note that the spacers 38 are formed on both ends of gate electrode G2 and on all sidewalls of cap oxide layer OX2, but a portion of the top surface of gate conductor G2 remains exposed, whereas the top surfaces and sidewalls of remaining gate conductors G1, G3 and G4 are encapsulated by the caps OX1, OX3 and OX4, as well as, the spacers 38 juxtaposed therewith. Also, the spacer 38 in trough 37 leaves a smaller trough 37' between gate electrode G2 and STI region 33C.
In step 68, in FIG. 5A, as shown a set of N+ source/drain regions S/D 35A, 35B, 35C, and 35D in FIG. 2D, are being formed in the P-substrate 31 between and adjacent to the spacers 38. Also, as shown in FIG. 3E, an N+ source/drain region 35E is being formed between STI region 33B and a spacer 38 in the P-substrate 31. In FIG. 3D, it should be noted that between gate electrode G2 and STI region 33C to the right there are no source/drain regions shown in the P-substrate 31 since the structure does not provide a window down to the substrate and the spacer 38 to the right of gate G2 extends down into the trough 37 formed to the right of the gate G2 blocking ion implantation into the substrate 31 there. In the case of an N-type doped substrate, then the ion implant will be a P+ dopant comprising BF 2 ions applied in a range from about 2E15 ions/cm -2 to about 6E15 ions/cm -2 at an energy from about 20 keV to about 60 keV. In the case of an P-type doped substrate, then the ion implant will be a N+ dopant comprising As ions applied in a range from about 2E15 ions/cm -2 to about 6E15 ions/cm -2 at an energy from about 25 keV to about 80 keV.
In step 70, in FIG. 5B as shown in FIGS. 2F and 3F a blanket silicon nitride (Si 3 N 4 ) etch stop layer 40 has been formed over the device 30 with a thickness from about 200 Å to about 600 Å.
Referring to FIGS. 2F and 3F, the device of FIGS. 2E and 3E is shown after formation over device 30 of a blanket Inter Layer Dielectric layer ILD composed of a PECVD TEOS glass layer with a thickness from about 1,000 Å to about 2,000 Å and a Boron Phosphorus TEOS glass layer with a thickness from about 3,000 Å to about 12,000 Å. (See Wolf, "Silicon Processing for the VLSI Era Vol. 2-Process Integration", (1990) Pages 195-196. Also see commonly assigned, U.S. Pat. No. 5,631,179 based upon application Ser. No. 08/511,062 filed Aug. 3, 1995 of H. C. Sung and L. Chen for "Method of Manufacturing Metallic Source Line, Self-Aligned Contact and Device Manufactured Thereby".
Referring again to FIGS. 2F and 3F, and to step 74, the device 30 is shown after heating the device to planarized the layer ILD by heating from about 750° C. to about 900° C. Next, as shown in step 76, there is an etch back of layer ILD to further planarize the layer ILD producing a thickness of layer ILD from about 2,000 Å to about 6,000 Å.
In step 78 a mask PR2 with windows W4 (FIG. 3F) and windows W3, W4, W5, and W6 (FIG. 2F) therethrough is formed over layer ILD to define Self-Aligned Contact (SAC) areas to source/drain regions 35A, 35B, 35C, 35D and 35E and to the gate conductor G2 to connect source and drain SAC areas and the butted contact BC1.
Referring to FIGS. 2G and 3G the device 30 of FIG. 2F and FIG. 3F is shown after performance of the etching step 80 (FIG. 5B) to form SAC areas wherein the device 30 has been etched the exposed portions of layer ILD through windows W3, W4, W5, and W6 in mask PR2 down to silicon nitride etch stop layer 40 to form openings spaces W3', W4', W5', and W6' to expose the SAC regions. The opening W4' through window W4 prepares for formation of a Self Aligned Butted Contact (SABTC), in accordance with this invention, at the left end of gate electrode G2. This provides for the SAC (ILD) etching with silicon nitride (Si 3 N 4 ) layer 40 providing the etch stop.
FIGS. 2H and 3H show the device of FIGS. 2G and 3G after the removal of silicon nitride layer 40 by dry etching with an etching gas such as CHF 3 and Oxygen (O 2 ). This leaves the surface of gate G2 exposed through opening space W4' enabling the formation of a butted contact BC1 thereto. It also exposes the surfaces of the N+ Source/Drain regions 35A, 35B, 35C, and 35D to provide the basis for forming SAC contacts therewith in succeeding manufacturing steps.
FIGS. 2I and 3I show the device of FIGS. 2H and 3H after the step 84 comprising formation of a pair of barrier metal--titanium and titanium nitride--layers 42 on the exposed surfaces of the substrate 31 and the sidewalls of layer ILD which are exposed. The barrier layers 42 are formed by formation of titanium to a thickness of about 300 Å covered with a layer of TiN to a thickness of about 1,000 Å.
Then in step 86 within the spaces defined by the barrier metal layers 42 are formed a set of tungsten plugs PL1, PL2, PL3 and PL4 which connect respectively to N+ Source/Drain regions 35A, 35B, 35C, and 35D and in the case of plug PL2, the lower right surface of the plug is in electrical and mechanical contact with gate G2 forming the SABTC contact adjacent to and in contact with gate G2 in accordance with this invention. The plugs PL1, PL2, PL3 and PL4 are formed by depositing a blanket layer of tungsten filling spaces W3', W4', W5', and W6'. The blanket tungsten layer is deposited to a thickness of about 5,000 Å above the surface of the device followed by etching back 5,000 Å leaving the plugs in the spaces W3', W4', W5', and W6' formed below windows W3, W4, W5, and W6 with a planarized surface with the tungsten plugs PL1, PL2, PL3 and PL4 planarized to be level with the substrate surface.
The combination of a Butted-contact with the SAC process results in a structure which take up less space which can also to connect drains of the pull down device and the gate of another pull down and pull up (PMOS) transistors.
Referring to step 88, the tungsten (W) plugs PL1, PL2, PL3 and PL4 are etched back to the surface of the Inter Layer Dielectric layer ILD.
In step 90, the back end of the line process steps are performed including defining Metal-1, forming vias, defining Metal-2 and forming passivation areas (include sputtering, photolithography and etching).
While this invention has been described in terms of the above specific embodiment(s), those skilled in the art will recognize that the invention can be practiced with modifications within the spirit and scope of the appended claims, i.e. that changes can be made in form and detail, without departing from the spirit and scope of the invention. Accordingly all such changes come within the purview of the present invention and the invention encompasses the subject matter of the claims which follow. | A method of forming a contact between a conductor and a substrate region in a MOSFET device is provided starting with forming a semiconductor substrate with a silicon oxide layer formed on the surface thereof. Then form a stack of a conductor material upon the surface of the silicon oxide layer and form a first dielectric layer upon the conductor material. Pattern the conductor stack into conductors. Form a butted contact pattern in the first dielectric layer by removal of the dielectric layer in at least one butted contact region. Form doped regions in the substrate self-aligned with the conductors. Form an etch stop layer over the device. Form a second dielectric layer over the device and pattern the second dielectric layer with contact openings therethrough down to the substrate and to the butted contact region. Employ the etch stop layer when patterning the second dielectric layer. Remove exposed portions of the etch stop layer subsequent to patterning the second dielectric layer. Form contacts to the substrate and the butted contact regions on the conductor through the contact openings. | 8 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] Not Applicable
STATEMENT AS TO RIGHTS TO INVENTIONS MADE UNDER FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
REFERENCE TO A “SEQUENCE LISTING,” A TABLE, OR A COMPUTER PROGRAM LISTING APPENDIX SUBMITTED ON A COMPACT DISK
[0003] Not Applicable
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] The present invention relates in general to semiconductor memories, and in particular, to apparatus and method for correcting duty cycle of clock signals used in semiconductor memories.
[0006] 2. Background of the Invention
[0007] Conventional duty cycle correction (DCC) technology can be classified into analogue DCC and digital DCC. Analogue DCC implementations tend to suffer from larger static current and narrower correction range for the duty cycle. On the other hand, analogue DCC typically provides higher resolution and therefore higher degree of correction, and are comparatively smaller in circuit size. In contrast, the drawbacks of the digital DCC are larger size and difficulty in significantly improving resolution. Moreover, digital DCC has a further disadvantage in that it is susceptible to noises occurring in the power supply. However, digital DCC merits are that it its static current is low, the correction process is rapid, and the correction range is wide. Due to such advantages, the digital DCC has been preferably utilized to correct clock signal duty cycle in semiconductor memory devices.
[0008] One type of digital DCC is disclosed in commonly owned copending application, U.S. Ser. No. 10/331,412, filed on Dec. 30, 2002, entitled “DIGITAL DLL APPARATUS FOR CORRECTING DUTY CYCLE AND METHOD THEREOF”, which is incorporated herein by reference. In such digital DCC, two delay lock loops (DLLs) are provided for the duty cycle correction. Because the DLL circuitry is nearly doubled in size (two phase mixers, two delay model units and two direct phase detectors), this implementation consumes larger silicon area.
[0009] Further, precise synchronization requires each of the two phase mixers, the two delay model units and the two direct phase detectors in each of the two delay lock loops to have substantially identical delay regardless of variations in process, voltage, temperature, etc. In such digital DCC, however, it is a challenge to match the phases of the two clocks used for each of the two delay lock loops accurately by equalizing each delay amount of the circuit elements, i.e., the phase mixers, the delay model units and the second direct phase detectors, involved in each delay lock loop.
BRIEF SUMMARY OF THE INVENTION
[0010] The present invention provides apparatus and method for implementing duty cycle correction that consumes relatively smaller silicon area.
[0011] The present invention also provides duty cycle correction apparatus and method capable of performing a more rapid phase lock.
[0012] The present invention further provides duty cycle correction apparatus and method capable of reducing the amount of current dissipation.
[0013] In accordance with an aspect of the present invention, there is provided a duty cycle correction apparatus for use in a semiconductor memory device, the apparatus including a delay line unit for delaying a first clock signal to produce a first delayed clock signal; an output tap unit for delaying the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal derived from a second clock signal; and a phase mixer for mixing the clock signal from the output tap unit and one of the first and second clock signals.
[0014] In accordance with another aspect of the present invention, there is provided a duty cycle correction apparatus for use in a semiconductor memory device including a delay line
[0015] In accordance with another aspect of the present invention, there is provided a duty cycle correction apparatus for use in a semiconductor memory device including a delay line unit for delaying a first clock signal to produce a first delayed clock signal; an output tap unit for delaying the first delayed clock signal by a pulse width of a first logic state of the first delayed clock signal, under the control of a toss control signal arranged at a rising edge of a first logic state of a second clock signal which is a complementary signal of the first clock signal, to produce a delay line output clock signal arranged at a falling edge of a first logic state of the first delayed clock signal; and a phase mixer for mixing a delay line output inversion clock signal inverted from the delay line output clock signal and the first clock signal.
[0016] In accordance with another aspect of the present invention, there is provided a duty cycle correction method for use in a semiconductor memory device including the steps of: (a) delaying a first clock signal to produce a first delayed clock signal; (b) delaying the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal generated from a second clock signal; and (c) mixing the clock signal from step (b) and one of the first and second clock signals.
[0017] In accordance with another aspect of the present invention, there is provided a duty cycle correction method for use in a semiconductor memory device including the steps of: (a) delaying a first clock signal to produce a first delayed clock signal; (b) delaying the first delayed clock signal by a pulse width of a first logic state of the first delayed clock signal under the control of a toss control signal arranged at a rising edge of a first logic state of a second clock signal, which is a complementary signal of the first clock signal, to produce a delay line output clock signal arranged at a falling edge of a first logic state of the first delayed clock; and (c) mixing a delay line output inversion clock signal inverted from the delay line output clock signal and the first clock signal.
[0018] In accordance with another aspect of the present invention, there is provided a semiconductor memory device having a delay lock loop (DLL) including a delay line unit for delaying a first clock signal related to a DLL output clock signal from the DLL, to produce a first delayed clock signal; an output tap unit to delay the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal derived from a second clock signal; a phase mixer to mix the clock signal from the output tap unit and one of the first and second clock signals; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals based on the second clock signal to generate phase control signals.
[0019] In accordance with another aspect of the present invention, there is provided a semiconductor memory device having a delay lock loop (DLL) including a delay line block that delays a first clock signal related to a DLL output clock signal from the DLL, to produce a first delayed clock signal; an output tap unit for delaying the first delayed clock signal by a pulse width of a second logic state of the first delayed clock signal, under the control of a toss control signal arranged at a rising edge of a first logic state of a second clock signal which is a complementary signal of the first clock signal, to produce a delay line output clock signal arranged at a falling edge of a first logic state of the first delayed clock signal; a phase mixer that mixes a delay line output inversion clock signal inverted from the delay line output clock signal and the first clock signal; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals, based on the second clock signal to generate phase control signals.
[0020] In accordance with another aspect of the present invention, there is provided a semiconductor memory device comprising a delay lock loop (DLL) having an input buffering block to buffer an externally input second clock signal, wherein the input buffering block includes: a delay line unit to delay a first clock signal, which is a complementary signal of the second clock signal, to produce a first delayed clock signal; an output tap unit to delay the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal generated from the second clock signal; a phase mixer to mix the clock signal from the output tap unit and one of the first and second clock signals; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals, based on the second clock signal, to generate phase control signals.
[0021] In accordance with another aspect of the present invention, there is provided a semiconductor memory device comprising a delay lock loop (DLL) having an input buffering block to buffer an externally input second clock signal, wherein the input buffering block includes: a delay line unit that delays a first clock signal, which is a complementary signal of the second clock signal, to produce a first delayed clock signal; an output tap unit that delays the first delayed clock signal by a pulse width of a first logic state of the first delayed clock signal, under the control of a toss control signal arranged at a rising edge of a first logic state of the second clock signal, to produce a delay line output clock signal arranged at a falling edge of a pulse of a first logic state of the first delayed clock signal; a phase mixer to mix a delay line output inversion clock signal inverted from the delay line output clock signal and the first clock signal; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals based on the second clock signal to generate phase control signals.
[0022] In accordance with another aspect of the present invention, there is provided a semiconductor memory device having a delay lock loop (DLL) including an input buffer to buffer an externally input second clock signal; a delay line unit for delaying a first clock signal, which is a complementary signal of the second clock signal, to produce a first delayed clock signal; an output tap unit for delaying the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal generated corresponding to the second clock signal; a phase mixer that mixes the clock signal from the output tap unit and one of the first and second clock signals, to thereby output a mixed clock signal onto a delay line within the DLL; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal, outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals based on the second clock signal to generate phase control signals.
[0023] In accordance with another aspect of the present invention, there is provided a semiconductor memory device having a delay lock loop (DLL) including an input buffer that buffers a second clock signal inputted from outside; a delay line unit for delaying a first clock signal, which is a complementary signal of the second clock signal, to produce a first delayed clock signal; an output tap unit that delays the first delayed clock signal by a pulse width of a first logic state of the first delayed clock signal, under the control of a toss control signal arranged at a rising edge of a first logic state of the second clock signal, to produce a delay line output clock signal arranged at a falling edge of a pulse of a first logic state of the first delayed clock signal; a phase mixer that mixes the clock signal from the output tap unit and one of the first and second clock signals, to thereby output a mixed clock signal onto a delay line within the DLL; a phase comparator that compares a phase of a duty cycle correction output clock signal with that of a duty cycle correction feedback clock signal outputted from the phase mixer, to provide phase comparison signals; and a phase mixer controller that counts the number of the phase comparison signals based on the second clock signal to generate phase control signals.
BRIEF DESCRIPTION OF THE DRAWINGS
[0024] The above and other objects and features of the present invention will become apparent from the following description of the preferred embodiments given in conjunction with the accompanying drawings, in which:
[0025] FIG. 1 is a block diagram showing a duty cycle correction device in accordance with one embodiment of the present invention;
[0026] FIG. 2 is a timing diagram describing an operation of the duty cycle correction device shown in FIG. 1 ;
[0027] FIG. 3 is a circuit diagram showing exemplary implementations for a delay line block and an output tap block shown in FIG. 1 ;
[0028] FIG. 4 is a detailed circuit diagram showing an exemplary implementation for a DCC phase mixer shown in FIG. 1 ;
[0029] FIG. 5 is a detailed circuit diagram depicting an exemplary implementation for a phase comparator shown in FIG. 1 ;
[0030] FIG. 6 is a detailed circuit diagram showing an exemplary implementation for the phase mixer controller shown in FIG. 1 ; and
[0031] FIG. 7 is a block diagram showing a duty cycle correction device in accordance with another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0032] Hereinafter, semiconductor memory devices in accordance with embodiments of the present invention are described in detail, with reference to the accompanying drawings.
[0033] FIG. 1 is a block diagram showing a duty cycle correction device in accordance with one embodiment of the present invention, and FIG. 2 is a timing diagram describing an operation of the duty cycle correction device shown in FIG. 1 .
[0034] The duty cycle correction device in accordance with the present invention comprises a delay line block 101 , a buffer 102 , an output tap block 103 , a DCC phase mixer 104 , a phase mixer controller 106 and a phase comparator 105 .
[0035] Specifically, delay line block 101 delays for a certain interval an external inversion clock signal clkb inverted from an external clock signal clk by an inverter. In the meantime, buffer 102 buffers external clock signal clk to thereby output a toss control signal toss-ctl.
[0036] Thereafter, output tap block 103 delays a phase of the external inversion clock signal clkb progressing along a delay line within delay line block 101 by a width of “H” pulse of clock signal clkb, in response to toss control signal toss-ctl from buffer 102 , to provide a delay line output clock signal DL_oclk.
[0037] DCC phase mixer 104 corrects a duty of the external clock signal clk using external inversion clock signal clkb and a delay line output inversion clock signal DL_oclkb that is obtained by inverting delay line output clock signal DL_oclk. Phase comparator 105 compares a phase of a DCC output clock signal DCC_oclk with that of a DCC feedback clock signal DCC_fbclk from DCC phase mixer 104 . Based on the comparison result at phase comparator 105 , phase mixer controller 106 outputs a signal for controlling a phase of the clock signal to DCC phase mixer 104 .
[0038] If the external inversion clock signal clkb is provided from a duty cycle correction device according to another embodiment of the present invention (not shown), then delay line block 101 delays external clock signal clk and buffer 102 buffers external inversion clock signal clkb to output toss control signal toss-ctl. At this time, DCC phase mixer 104 can input external clock signal clk and delay line output clock signal DL_oclk and mix phases of both clock signals. In this case, an output clock from DCC phase mixer 104 is the reverse of a phase of the clock signal DCC_oclk shown in FIG. 2 .
[0039] FIG. 3 is a circuit diagram showing an exemplary implementation for delay line block 101 and output tap block 103 of FIG. 1 .
[0040] As shown, output tap block 103 , in response to the toss control signal toss-ctl from buffer 102 , delays a phase of external inversion clock signal clkb propagating along a delay line within delay line block 101 by “H” pulse width of clock signal clkb, and generates delay line output clock signal DL_oclk. That is, during the external inversion clock signal clkb of rising edge moves along the delay line within delay line block 101 . When the toss control signal toss-ctl is transited to a logic “H,” the signal clkb can be outputted to output tap block 103 . According to one embodiment of the invention shown in FIG. 1 , an inverter can be coupled to an output port of output tap block 103 . Further, according to another embodiment of the present invention, it can also be embedded within output tap block 103 . According to still another embodiment of the invention, the inverter can be installed within phase mixer 104 . It should be noted that even though there are presented only several embodiments, as above, for simplification, the invention is not limited to those embodiments.
[0041] In the duty cycle correction device, toss control signal toss-ctl can be a signal arranged at a rising edge of the “H” pulse of the external clock signal clk. Further, according to another embodiment of the invention, toss control signal toss-ctl can be a signal arranged at a falling edge of the “H” pulse of the external inversion clock signal clkb. Moreover, referring to FIG. 2 , a pulse width of toss control signal toss-ctl is substantially identical to that of external clock signal clk. When toss control signal toss-ctl is arranged at a rising edge of “H” pulse of the external clock signal clk, the toss control signal can be enabled to a logic “H” state. If the toss control signal toss-ctl is logic “L” state, then outputs of 3 input NAND gates constituting respective output taps within output tap block 103 are all in logic “H” state. According to the above, external inversion clock signal clkb propagates within delay line block 101 . By the progress of external inversion clock signal clkb, an output of the delay line transitions from logic “L” state to logic “H” state. The operation of a unit delay cell (hereinafter, referred as “UDC”) within line delay block 101 and individual output taps within output tap block 103 are described with reference to Table. 1 below:
TABLE 1 No. of UDC 301 302 303 Timing t − 1 T t + 1 3-input of NAND toss-ctl H H H gate Present UDC H H L Inverting the L H L Next UDC
[0042] As can be seen from Table. 1, if the rising edge of the external inversion clock signal clkb passes through a present UDC 302 , the output of 3-input NAND gate becomes logic state “L”. The output of the 3-input NAND gate turns on a transmission gate within an output tap 312 , and then is provided as the delay line output clock signal DL_oclk. Consequently, the rising edge of the delay line output clock signal DL_oclk can be synchronized with the falling edge of the external clock signal clk.
[0043] In accordance with this aspect of the present invention, DCC phase mixer 104 mixes a phase of the external inversion clock clkb and that of delay line output inversion clock signal DL_oclk inverted from delay line output clock signal DL_oclk, thereby correcting a duty of external clock signal clk.
[0044] Further, in accordance with another embodiment of the invention, DCC mixer 104 can receive external clock signal clk and delay line output clock signal DL_oclk and mix phases of the both clock signals. In this case, the output clock signal from DCC phase mixer 104 is a complementary one of the clock shown in FIG. 2 .
[0045] However, since, with only the structure as described above, the desirable output cannot be derived from DCC phase mixer 104 , it is preferable that the duty cycle correction device in accordance with the exemplary embodiment of the invention described herein comprises phase comparator 105 and phase mixer controller 106 .
[0046] FIG. 5 is a detailed circuit diagram depicting an exemplary implementation for phase comparator 105 shown in FIG. 1 .
[0047] As shown, phase comparator 105 of the present invention compares a phase of DCC output clock signal DCC_oclk with that of DCC feedback clock signal DCC_fbclk from phase mixer 104 , to output phase comparison signals, s 1 _Inc, s 1 _Dec, s 2 _Inc and s 2 _Dec. If a duty ratio of external clock signal clk is larger than 50%, then a phase of a rising edge of DCC output clock signal DCC_oclk lags behind a rising edge of the DCC feedback clock. In this case, phase comparator 105 causes a phase control signal s 1 to increase and phase control signal s 2 to decrease. But if the duty ratio of the external clock signal clk is smaller than 50%, then a phase of a rising edge of the DCC output clock signal DCC_oclk precedes a rising edge of the DCC feedback clock DCC_fbclk. In this case, phase comparator 105 allows phase control signal s 1 to decrease and phase control signal s 2 to increase.
[0048] Phase mixer controller 106 , as shown in FIG. 6 , can comprise a plurality of counters of N bits which output phase control signals, s 1 _ 1 to s 1 _N and s 2 _ 1 to s 2 _N, by counting the clock being inputted, using the phase comparison signals, s 1 _Inc, s 1 _Dec, s 2 _Inc and s 2 _Dec. That is, it sequentially increases and decreases the number of phase control signals, s 1 _ 1 to s 1 _N, activated by the phase comparison signals, s 1 _Inc and s 1 _Dec. In the same manner, it sequentially increases and decreases the number of phase control signals, s 2 _ 1 to s 2 _N, activated in response to the phase comparison signals s 2 _Inc and s 2 _Dec. Thereafter, as shown in FIG. 4 , DCC phase mixer 104 can mix the phase of the external inversion clock signal clkb and that of the delay line output inversion clock signal DL_oclkb.
[0049] Now, concrete operational examples in accordance with present invention are presented below. First, assume that the phase of external inversion clock signal clkb comes before that of delay line output inversion clock signal DL_oclkb. Due to the phase difference, the first counter in phase mixer controller 106 activates first to third upper phase control signals, s 1 _ 1 to s 1 _ 3 , and the second counter activates a first lower phase control signal s 2 _ 1 . After doing so, DCC phase mixer 104 shown in FIG. 4 mixes the phase of external inversion clock signal clkb and the phase of delay line output inversion clock signal DL_oclkb by the high impedance inverter. This generates a mixed clock signal at a position of ¼ from the preceding clock signal.
[0050] In the meantime, as another embodiment of the phase mixer controller 106 , can be designed in a manner such that any one of the phase control signals, s 1 _ 1 to s 1 _N, is activated and any one of the phase control signals, s 2 _ 1 to s 2 _N, is activated. For this, the high-impedance inverters in DCC phase mixer 104 of FIG. 4 must be designed at a different size. In other words, because the phase difference is large, the size of the high-impedance inverters turned-on in response to the phase control signals becomes large. Further, there is a method that can be used that combines a plurality of high-impedance inverters in serial and parallel, while maintaining the size of the high-impedance inverters in the DCC phase mixer 104 of FIG. 4 identically. In the above embodiment, there can be further methods where the high-impedance inverters in DCC phase mixer 104 are designed in a different sizes. However, their detailed descriptions are omitted herein for simplification.
[0051] FIG. 7 is a block diagram showing a duty cycle correction device in accordance with another embodiment of the present invention, wherein the input signal is different from the embodiment shown in FIG. 1 . That is to say, as shown in another embodiment of FIG. 7 , the external clock signal clk and the inversion clock signal clkb are received directly from the outside.
[0052] A duty cycle correction device of the present invention having such configuration can be operated by a connection with an output port of the delay lock loop. Otherwise, the inventive duty cycle correction device can be operated by a connection with an input port of the delay lock loop. That is, it can be employed in the clock input buffer. Alternatively, the inventive duty cycle correction device can be operated by positioning it between the clock input buffer and the delay lock loop.
[0053] As a result, the present invention can considerably reduce the size of duty cycle correction devices while reducing power consumption. Further, the invention can considerably decrease time taken to perform duty cycle correction. In other words, the duty cycle correction operation using a conventional delay lock loop is made during a stable period of approximately dozens to 200 cycles. However, according to the duty cycle correction device of the present invention employing the novel delay lock loop, the correction operation can be made during only a single cycle.
[0054] The present application contains subject matter related to Korean patent application No. 2004-28975, filed in the Korean Patent Office on Apr. 27, 2004, the entire contents of which are incorporated herein by reference.
[0055] As described above, although the present invention is explained by specific embodiments and drawings, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. | The present invention is directed to a duty cycle correction apparatus that can be implemented in a small size, and is capable of performing a phase lock more rapidly, and reducing the amount of current being consumed, and to a method thereof. The duty cycle correction apparatus in accordance with the present invention for use in a semiconductor memory device includes a delay line unit for delaying a first clock signal to produce a first delayed clock signal; an output tap unit for delaying the first delayed clock signal by a pulse width of a first logic state of the first clock signal under the control of a toss control signal derived from a second clock signal; and a phase mixer for mixing the clock signal from the output tap unit and one of the first and second clock signals. | 7 |
FIELD OF THE INVENTION
The invention relates to a cable connector assembly comprising cover means and connecting means, said cover means comprising wall portions and an opening adapted to accommodate said connecting means.
BACKGROUND OF THE INVENTION
WO 99/27616 discloses a high density electrical connector system, wherein the electrical connectors have a hood with a sloping top. Because of the slope of the hood and the position of the opening in the hood for a cable, a second connector does not interfere with this cable.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a cable connector assembly and a connector system wherein cable management is facilitated. This is important since the cabinets containing the cables are getting smaller and the density of cable connector assemblies on a circuit board increases.
This object is achieved by providing a cable connector assembly characterized in that at least one of said wall portions is at least partially curved for guiding at least one cable of at least one other cable connector. By adapting the cover means such that it allows guiding cables of other cable connector assemblies, these cables can be controlled by the cover means. The curvature of the wall portion can be close to the minimum bend radius at which a signal through the guided cable or the shielding of the cable starts to degrade. For the shielding of the cable, especially the braid is susceptive for bend forces if the bend radius of the cable becomes too small.
In an embodiment of the invention the cover means of the cable connector has means for reducing the movement of a cable over the cover means. Preferably these means include cable tie means for attaching the cable to the partially curved wall portion to secure the guided cable. Alternatively or in addition the curved wall portion may be curved substantially perpendicular to a longitudinal axis of the curved wall portion. This is e.g. advantageous if a single cable is to be guided over the curved wall portion. Moreover other structures or material compositions for the wall portion can be envisaged that are adapted to reduce the movement of the cable.
can be envisaged that are adapted to reduce the movement of the cable.
The invention also relates to a cable connector system comprising at least a first and a second cable connector assembly according to any one of the preceding claims, wherein said first cable connector comprises said at least partially curved wall portion and said second cable connector comprises a wall portion having an opening adapted for directing said cable substantially tangential to said at least partially curved wall portion. By adapting the opening the cable connectors can be positioned in close proximity to each other, thereby providing the possibility to obtain a high density system of cable connectors on e.g. a circuit board with improved cable management features. The system may comprise several cable connector assemblies, wherein the cover means of the assemblies guide at least some of the cable of these cable connector assemblies. These cables can be attached to the cover means by cable tie means. In this way a flexible cable management system is obtained.
The invention also relates to the cover means as such, comprising an at least partially curved wall portion.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will be further illustrated with reference to the attached drawing, which shows a preferred embodiment according to the invention. It will be understood that the cable connector assembly and system according to the invention are not in any way restricted to this specific and preferred embodiment.
FIG. 1 shows a cable connector system according to an embodiment of the invention;
FIG. 2 shows a perspective view of a cable connector assembly according to a first embodiment of the invention.
FIG. 3 shows different cable clamp arrangements;
FIGS. 4A and 4B show perspective views of two parts of a cover according to a second embodiment of the invention;
FIGS. 5A and 5B show perspective views of a cable connector assembly according to a second embodiment of the invention;
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a cable connector system 1 comprising a first cable connector assembly 2 and a second cable connector assembly 3 on a printed circuit board 4 . Each of said assemblies 2 , 3 has a cable 5 extending from said assemblies 2 , 3 . In FIG. 1 only the cover means 6 , 7 of respectively the assemblies 2 and 3 are visible. It is noted that cover 6 and 7 may be identical or similar. The cover means 6 , 7 , hereinafter also referred to as cover, comprises upper wall portions 8 , 9 that are curved for guiding the cable 5 . The curvature of the upper wall is preferably close to the minimum bend radius of the cable 5 . As a general rule the bend radius of the curved wall portion 8 , 9 is equal to or higher than five times the outer diameter of the cable. For instance, in a cable connector system 1 with three types of cables 5 with outer diameters of 5 , 6.5 and 10 mm, the curvature of the wall portions 8 , 9 of the cover means 6 , 7 is adapted to the cable 5 with the largest diameter, i.e. the curvature of the wall portions 8 , 9 is at least 50 mm.
The cable 5 is reduced in movement and assisted in guidance by the cable tie 10 that attaches cable 5 . This cable tie 10 may e.g. be of plastic material and can be adapted to easily fasten and release a cable. Alternatively the cable tie 10 may be a metal or plastic cable clamp. The cable tie 10 may be integrated with the cover means 6 , 7 . Cable tie 10 may attach several cables 5 from other connector assemblies (not shown) as well. The covers 6 , 7 comprise a recess or slot 11 for holding the cable tie 10 . It is noted that the recess 11 for the cable tie 10 is not necessarily located near the position on the upper wall where the cable approaches the assembly, but may e.g. be located in the middle of the upper wall 8 , 9 . Also more than one cable tie 10 can be applied.
The assemblies 2 , 3 further comprise cable openings 12 (see FIG. 2 ) that are e.g. adapted by the alignment part 13 to direct the cable 5 of assembly 2 tangential to the curved wall portion 9 of the assembly 3 . To facilitate this alignment an alignment part 13 may have a direction which gives cable 5 a direction which is just below the tangential direction such that contact with the upper wall 9 is ensured. Alignment parts 13 and the tie-wraps 14 may also have a bend relief function in FIG. 1 . Alignment part 13 may be an integral part of the cover 6 , 7 as well as being a mountable part. The upper wall 9 may comprise a small linear part near the location where the cable 5 meets the cover 7 to define the tangential direction for the cable 5 . The cables 5 can be attached to the covers 6 , 7 by the tie wrap 14 . The assemblies 2 , 3 are fastened to the printed circuit board 4 with screws 15 . Covers 6 and 7 are provided with indents 16 for fingers to facilitate unmating of the connector assemblies 2 , 3 from the headers (not shown) of the printed circuit board 4 .
The construction of a cable connector assembly 2 , 3 according to two embodiments of the invention will be discussed next in greater detail.
FIG. 2 shows a perspective view of the connector assembly 2 wherein the front part of the cover 6 is removed. Cover 6 comprises sidewall portions 20 , 21 and 22 that together with the front part side wall 23 (see FIG. 4B ) of the cover determine an opening 24 opposite to the partially curved upper wall 8 , which opening 24 accommodates connecting means or terminal blocks 25 to be mounted on the printed circuit board 4 . The front part of the cover 6 can be attached to the assembly 2 by using pins 26 . Cable opening 12 may comprise a cable clamp 27 inserted in a slot of the cover 6 for strain relief of the cable 5 . A connector assembly 2 may have several cables 5 , possibly of different diameters, connected to the terminal blocks 25 . Therefore different cable clamps 27 ′, 27 ″ can be used, as shown in FIG. 3 . The several cables 5 may all be guided by the upper wall 9 of cable assembly 3 or, alternatively, some of the cables 5 leaving cable assembly 2 are guided by the upper wall 9 .
FIGS. 4A and 4B show perspective views of two parts 30 and 31 that are to be attached to each other to form a cover 6 . Similar or equivalent parts of the covers with respect to the first embodiment have been assigned identical reference numbers. The alignment part 13 at the cable opening 12 shown in FIG. 2 is omitted in the second embodiment. Instead the sidewalls 21 , 23 of the cover 6 comprise a structure 32 forming a tubular cable opening 12 when the sidewalls 21 and 23 are attached to each other by fitting the pins 26 in corresponding holes 33 . This tubular cable opening is adapted to perform the same function as the alignment part 13 in FIG. 2 .
In FIG. 5A the cable assembly 2 is shown comprising a cable 5 in the tubular cable opening 12 formed by the structure 32 in the sidewall 21 of the cover 6 . Cable 5 comprises a plurality of wires 34 that are to be connected to the appropriate terminal blocks 25 . The cable 5 can be attached to the cover 6 in the tubular cable opening 12 by one or more components 35 for fixation of the cable to the cover 6 . Such a component 35 may be a wrap that can be shrunk around the cable 5 and fitted in the tubular opening 12 . Component 35 has a similar function as the cable clamps 27 , 27 ′, 27 ″ as shown in FIG. 3 . In FIG. 5B the connector assembly 2 is shown with the sidewall 23 in place, ready to be mounted to a printed circuit board 4 . When mounted cable 5 can be guided by the upper walls of other similar connector assemblies, such as connector assembly 3 . In this way management of the cables is improved.
It is noted that the cable or cables 5 of the connector assemblies 2 , 3 are not necessarily in contact with the entire upper wall 8 , 9 . Especially at the end of the curved upper wall, the cable 5 may diverge from the upper wall since e.g. the destination of the cable 5 urges this cable to a particular direction.
Moreover it is noted that alternatively or in addition to the cable tie 10 , other means for reducing movement and/or assisting the guidance of the cable 5 can be applied on the upper wall 8 , 9 . E.g. the upper wall 8 , 9 may comprise a groove or further curvature in the longitudinal direction of the upper wall 8 , 9 . Further, structures or material compositions of or on top of the upper wall 8 , 9 that are able to exert a sufficient friction force to the cable 5 when moved can be envisaged as well. | The invention relates to a cable connector assembly including cover means and connecting means, wherein the cover means include wall portions and an opening adapted to accommodate the connecting means. At least one of the wall portions is at least partially curved for guiding at least one cable of one or more other cable connector assemblies. Cable ties to attach the cable to the curved wall portion are disclosed are well. The invention facilitates cable management in dense and small cabinets. | 8 |
FIELD OF THE INVENTION
[0001] This invention relates to a reactor, and more particularly to a chemical vapor deposition reactor.
BACKGROUND OF THE INVENTION
[0002] Chemical vapor deposition is a thin film deposition technique about using a method of depositing a solid product onto a chip surface from reactants by a chemical reaction in a reactor. The reactants are usually gas reactants. After decades of developments, the chemical vapor deposition has become the most important and the main deposition method in the semiconductor manufacturing process for depositing a thin film on the semiconductor elements, such as conductors, semiconductors, and dielectric materials.
[0003] The key equipment of the facilities for chemical vapor deposition is a reactor, where is the place for deposing a thin film. However, the designs for chemical vapor deposition reactors are different from one another according to their application scopes. A Hydrogen Vapor Phase Epitaxy reactor, HVPE reactor, is one of the popular chemical vapor decomposition reactors.
[0004] The conventional HVPE reactors for growth of compound semiconductors of IV and III-V groups of periodical table and their alloys are well-known in the industry. These reactors can be divided into three main groups according to their geometrical features. The three main groups are respectively HVPE reactors with horizontal geometry of gas flow (HG HVPE reactors), HVPE reactors with vertical geometry of gas flow (VG HVPE reactors), and HVPE reactors with close shower head (SH HVPE reactors).
[0005] Please refer to FIG. 1, which shows a structural diagram of a prior HG HVPE reactor. As shown in FIG. 1, the HG HVPE reactor includes a horizontal tube 11 , a horizontal reagent gas flow 12 , a substrate 13 , and a gas heater 14 . A hydride thin film is deposited on the substrate 13 through a reaction of the horizontal reagent gas flow 12 in the HG HVPE reactor. The relevant structures and features of HG HVPE reactors are disclosed in U.S. Pat. Nos. 6,176,925, 6,177,292, 6,179,913 and 6,350,666.
[0006] The disadvantages of above-mentioned HG HVPE reactors include: 1. It's difficult to obtain a high efficiency of gas utilization and high growth uniformity of the thin film simultaneously. 2. A big gas heater 14 with high power consumption is necessary to avoid the temperature gradients inside the horizontal tube 11 . 3. Because it is difficult to obtain the temperature difference between the reactor inside walls and the substrate 13 , a deposition material will be deposited onto the reactor inside walls. 4. Because of the high relaxation times of temperature and gas flow rate changes, a Quantum Well structure, QW structure, is unable to be grown. 5. Because the symmetry of the reactor is low, it is difficult to control and model the growth processes of the thin film.
[0007] Please refer to FIG. 2, which shows a structural diagram of a prior VG HVPE reactor. As shown in FIG. 2, the VG HVPE reactor includes a vertical tube 21 , a vertical reagent gas flow 22 , a substrate 23 , and a gas heater 24 . A hydride thin film is deposited on the substrate 23 through a reaction of the vertical reagent gas flow 22 in the VG HVPE reactor. The relevant structures and features of VG HVPE reactors are disclosed in U.S. Pat. Nos. 5,980,632 and 6,086,673.
[0008] The disadvantages of above-mentioned VG HVPE reactors include: 1. The growth uniformity of the thin film is not yet ideal enough. 2. A big gas heater 24 with high power consumption is still necessary to avoid the temperature gradients inside the vertical tube 21 . 3. Because it is still difficult to obtain the temperature difference between the reactor inside walls and the substrate 23 , a deposition material will be deposited onto the reactor inside walls. 4. Because of the high relaxation times of temperature and gas flow rate changes, a Quantum Well structure, QW structure, is either unable to be grown.
[0009] Please refer to FIG. 3, which shows a structural diagram of a prior SH HVPE reactor. As shown in FIG. 3, the SH HVPE reactor includes a horizontal tube 31 , a vertical reagent gas flow 32 , a substrate 33 , a gas heater 34 , and a shower-type head 35 . A hydride thin film is deposited on the substrate 33 through a reaction of the vertical reagent gas flow 32 in the SH HVPE reactor. The SH HVPE reactor further includes a horizontal gas flow 36 as a buffer gas. The relevant structures and features of SH HVPE reactors are disclosed in U.S. Pat. No. 4,574,093.
[0010] The disadvantages of above-mentioned SH HVPE reactors include: 1. The sprinkle nozzle 35 is a non-technological design, so that the sprinkle nozzle 35 is difficult to be fabricated practically. 2. Because it is difficult to obtain the temperature difference between the reactor inside walls and the substrate 33 , deposition materials are deposited onto the reactor inside walls and the sprinkle nozzle 35 .
[0011] As above-mentioned, a HVPE reactor with the abilities of high efficiency of gas utilization and high growth uniformity of thin film, which avoids the erroneous deposition, is worthy for the relevant industries.
[0012] Because of the technical defects described above, the applicant keeps on carving unflaggingly to develop a “CHEMICAL VAPOR DEPOSITION REACTOR” through wholehearted experience and research.
SUMMARY OF THE INVENTION
[0013] It is an object of the present invention to provide a HVPE reactor with the advantages of being able to obtain high efficiencies of gas utilization and high growth uniformity of the thin film simultaneously.
[0014] It is another object of the present invention to provide a HVPE reactor with opposite direction flow geometry and extended diffusion layer. Also, a quantum well structure can be formed on a semiconductor material in the HVPE reactor.
[0015] It is the other object of the present invention to provide a HVPE reactor with a small volume and low power consumption.
[0016] In accordance with one aspect of the present invention, a reactor is provided for depositing a thin film on at least a substrate through a reaction between a vertical input reagent gas flow and the at least a substrate. A vertical output reagent gas flow is produced after the reaction. The reactor includes a vertical tube, at least a reaction chamber located inside the vertical tube, an input flow baffle located on the at least a reaction chamber, and at least a gas exit installed on the at least a reaction chamber for exhausting the vertical input reagent gas flow and the vertical output reagent gas flow. In addition, the substrate is located at the bottom of the at least a reaction chamber.
[0017] Preferably, the reactor is a hydride vapor deposition reactor.
[0018] Preferably, the input flow baffle is located on a top of the at least a reaction chamber.
[0019] Preferably, the at least a gas exit is installed on a side wall of the at least a reaction chamber.
[0020] Preferably, the reactor is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics.
[0021] Preferably, the vertical input reagent gas flow is a mixture of HCl, GaCl, NH 3 , and Ar gases.
[0022] Preferably, the substrate is a sapphire substrate.
[0023] Preferably, the thin film is one compound semiconductor selected from a group consisting of IV group and their alloys, III-V groups and their alloys, and GaN.
[0024] Preferably, the vertical output reagent gas flow is a mixture of HCl, GaCl, Cl 2 , NH 3 , and H 2 gases.
[0025] Preferably, the reactor further has an extended diffusion layer formed from a bottom of the reaction chamber to the gas exit for increasing a utility rate of the vertical input reagent gas flow and a deposition unity.
[0026] Preferably, the vertical tube includes a first gas heater and a second gas heater.
[0027] Preferably, the first gas heater is one of an external side wall gas heater and an internal side wall gas heater.
[0028] Preferably, the second gas heater controls a temperature difference between the substrate and walls of the reactor.
[0029] Preferably, the second gas heater is an external bottom gas heater.
[0030] Preferably, the second gas heater includes an input gas tube and a heater.
[0031] Preferably, the reaction chamber is a cylindrical chamber.
[0032] Preferably, the reactor further includes an extended diffusion layer for transport of the vertical input reagent gas flow to the substrate.
[0033] In accordance with another aspect of the present invention, a hydride vapor deposition reactor is provided for depositing a thin film on a substrate through a reaction between a vertical input reagent gas flow and the substrate. A vertical output reagent gas flow is produced after the reaction. The reactor includes a vertical tube with two side wall gas heaters and a bottom gas heater, a plurality of first input flow baffles located inside the vertical tube for extending routes of the vertical input reagent gas flow and the vertical output reagent gas flow, a reaction chamber located inside the vertical tube and upon the substrate, at least a second input flow baffle located on a top of the reaction chamber, and at least a gas exit installed on a side wall of the reaction chamber for exhausting the vertical input reagent gas flow and the vertical output reagent gas flow.
[0034] Preferably, the thin film is one compound semiconductor selected form a group consisting of III-V groups and their alloys, IV groups and their alloys, and GaN.
[0035] Preferably, the two side wall gas heaters are a first gas heater and a second gas heater respectively located on external side walls of the vertical tube.
[0036] Preferably, the vertical tube further includes a Ga vessel.
[0037] Preferably, the reactor further includes an extended diffusion layer formed from a bottom of the reaction chamber to the gas exit for increasing a utility rate of the vertical input reagent gas flow and a deposition unity.
[0038] Preferably, the plural first input flow baffles are located above the reaction chamber.
[0039] For understanding this application further, some figures and detailed illustrations are shown as follows:
BRIEF DESCRIPTION OF THE DRAWINGS
[0040] [0040]FIG. 1 shows a structural diagram of a prior HG HVPE reactor;
[0041] [0041]FIG. 2 shows a structural diagram of a prior VG HVPE reactor;
[0042] [0042]FIG. 3 shows a structural diagram of a prior SH HVPE reactor;
[0043] [0043]FIG. 4 shows a structural diagram of the HVPE reactor according to a preferred embodiment I of the present invention;
[0044] [0044]FIG. 5 shows a structural diagram of the HVPE reactor according to a preferred embodiment II of the present invention;
[0045] [0045]FIG. 6 shows a structural diagram of the HVPE reactor according to a preferred embodiment III of the present invention;
[0046] [0046]FIG. 7 shows a structural diagram of the HVPE reactor according to a preferred embodiment IV of the present invention;
[0047] [0047]FIG. 8 shows a structural diagram of the HVPE reactor according to a preferred embodiment V of the present invention; and
[0048] [0048]FIG. 9 shows a structural diagram of the HVPE reactor according to a preferred embodiment VI of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0049] The present invention provides HVPE reactors with opposite direction flow geometries and extended diffusion layers. And, a quantum well structure can be formed on a semiconductor material in the HVPE reactor.
[0050] Please refer to FIG. 4, which shows a structural diagram of a HVPE reactor according to the preferred embodiment I of the present invention. As shown in FIG. 4, the HVPE reactor includes a vertical tube 41 , a first gas heater 45 , a second gas heater 46 , a reaction chamber 47 , at least an input flow diaphragm 49 , and at least a gas exist slit 410 . The reaction chamber 47 includes a container space 48 . And, a substrate 43 for being deposited thereon is positioned at the bottom of the container space 48 .
[0051] The first gas heater 45 is positioned on the external side wall of the vertical tube 41 , and the second gas heater 46 is positioned at the external bottom wall of the vertical tube 41 . The reaction chamber 47 is located inside the vertical tube 41 and is a cylindrical reaction chamber. The input flow diaphragm 49 is positioned on the top of the reaction chamber 47 , and the at least a gas exist slit 410 is located on the internal side wall of the reaction chamber 47 with a particular distance from the substrate 43 . An extended diffusion layer 411 is formed between the height of the at least a gas exist slit 410 and the bottom of the reaction chamber 47 . The reaction chamber 47 is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrate 43 is a sapphire substrate.
[0052] The HVPE reactor of the preferred embodiment I is used for depositing the thin film 412 on the substrate 43 by a reaction between the vertical input reagent gas flow 42 and the substrate 43 . And, an opposite-direction vertical output reagent gas flow 44 is produced after the reaction. The vertical input reagent gas flow 42 and the vertical output reagent gas flow 44 can be exhausted through the gas exist slit 410 .
[0053] The vertical input reagent gas flow 42 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 412 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 44 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases. And, the second gas heater 46 is used for controlling the temperature difference between the substrate 43 and the internal side walls of the reactor.
[0054] On the other hand, the substrate 43 is not directly reacted with the vertical input reagent gas flow 42 . The reaction is proceeded during the diffusion process of the vertical input reagent gas flow 42 in the extended diffusion layer 411 . Meanwhile, the vertical input reagent gas flow 42 is still in a gas state during the diffusion process. Because the second gas heater 46 can be used to control the temperature difference between the internal side walls of the reactor and the substrate 43 , no deposition will be formed on the internal side walls of the reactor.
[0055] Therefore, the advantage of the reactor according to the preferred embodiment I is that the first gas heater 45 and the second gas heater 46 are not necessary to be sealed up, because they are not directly exposed to the vertical input reagent gas flow 42 and the vertical output reagent gas flow 44 . This reduces the reactor volume effectively.
[0056] Please refer to FIG. 5, which shows a structural diagram of a HVPE reactor according to the preferred embodiment II of the present invention. As shown in FIG. 5, the HVPE reactor includes a vertical tube 51 , a first gas heater 55 , a second gas heater 56 , a reaction chamber 57 , at least an input flow diaphragm 59 , and at least a gas exist slit 510 . The reaction chamber 57 includes a container space 58 . And, a substrate 53 for being deposited thereon is positioned at the bottom of the container space 58 .
[0057] The first gas heater 55 is positioned on the internal side wall of the vertical tube 51 and upon the input flow diaphragm 59 . The second gas heater 56 is positioned at the external bottom of the vertical tube 51 . The reaction chamber 57 is located inside the vertical tube 51 and is a cylindrical reaction chamber. The input flow diaphragm 59 is positioned on the top of the reaction chamber 57 , and the at least a gas exist slit 510 is located on the internal side wall of the reaction chamber 57 with a particular distance from the substrate 53 . An extended diffusion layer 511 is formed from the height of the at least a gas exist slit 510 to the bottom of the reaction chamber 57 . The reaction chamber 57 is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrate 53 is a sapphire substrate.
[0058] The HVPE reactor of the preferred embodiment II is used for depositing a thin film 512 on the substrate 53 by a reaction between the vertical input reagent gas flow 52 and the substrate 53 . And, an opposite-direction vertical output reagent gas flow 54 is produced after the reaction. The vertical input reagent gas flow 52 and the vertical output reagent gas flow 54 can be exhausted through the gas exist slit 510 .
[0059] The vertical input reagent gas flow 52 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 512 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 54 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases. And, the second gas heater 56 is used for controlling the temperature difference between the substrate 53 and the internal side walls of the reactor.
[0060] On the other hand, the substrate 53 is not directly reacted with the vertical input reagent gas flow 52 . The reaction is proceeded during the diffusion process of the vertical input reagent gas flow 52 in the extended diffusion layer 511 . Meanwhile, the vertical input reagent gas flow 52 is still in a gas state during the diffusion process. Because the second gas heater 56 can be used to control the temperature difference between the internal side walls of the reactor and the substrate 53 , no deposition will be formed on the internal side walls of the reactor.
[0061] The first gas heater 55 is directly exposed to the vertical output reagent gas flow 54 , so that the first gas heater 55 of the HVPE reactor of the preferred embodiment II needs to be sealed up. Furthermore, the advantage of the HVPE reactor according to the preferred embodiment II is more sensitive to the temperature change than the HVPE reactor of the preferred embodiment I.
[0062] Please refer to FIG. 6, which shows a structural diagram of a HVPE reactor according to the preferred embodiment III of the present invention. As shown in FIG. 6, the HVPE reactor includes a vertical tube 61 , a first gas heater 65 , a second gas heater 66 , a reaction chamber 67 , at least an input flow diaphragm 69 , and at least a gas exist slit 610 . The reaction chamber 67 includes a container space 68 . And, a substrate 63 for being deposited thereon is positioned at the bottom of the container space 68 .
[0063] The first gas heater 65 is positioned on the internal side wall of the vertical tube 61 and upon the input flow diaphragm 69 . The second gas heater 66 is positioned at the external bottom of the vertical tube 61 . The reaction chamber 67 is located inside the vertical tube 61 and is a cylindrical reaction chamber. The input flow diaphragm 69 is positioned on the top of the reaction chamber 67 , and the at least a gas exist slit 610 is located on the internal side wall of the reaction chamber 67 with a particular distance from the substrate 63 . An extended diffusion layer 611 is formed from the height of the at least a gas exist slit 610 to the bottom of the reaction chamber 67 . The reaction chamber 67 is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrate 63 is a sapphire substrate.
[0064] Particularly, the second gas heater 66 includes an input gas tube 612 and an internal heater 613 . A input reagent gas flow 614 is heated by the internal heater 613 while being flown through the input gas tube 612 . An output reagent gas flow 615 is formed after the heated input reagent gas flow 614 is reflected from the bottom of the substrate 63 . The input reagent gas flow 614 and the output reagent gas flow 615 are oppositely directed and thermally coupled. Because the temperature of the substrate 63 directly depends on the heated input reagent gas flow 614 , the temperature can be changed quickly.
[0065] The HVPE reactor of the preferred embodiment III is used for depositing a thin film 616 on the substrate 63 by a reaction between the vertical input reagent gas flow 62 and the substrate 63 . And, an opposite-direction vertical output reagent gas flow 64 is produced after the reaction. The vertical input reagent gas flow 62 and the vertical output reagent gas flow 64 can be exhausted through the gas exist slit 610 .
[0066] The vertical input reagent gas flow 62 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 616 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 64 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases.
[0067] In the preferred embodiment III, the substrate 63 is not directly reacted with the vertical input reagent gas flow 62 . The reaction is proceeded during the diffusion process of the vertical input reagent gas flow 62 in the extended diffusion layer 611 . And, the vertical input reagent gas flow 62 is still in a gas state during the diffusion process. The second gas heater 66 is used for controlling the temperature difference between the substrate 63 and the internal side walls of the reactor, so that no deposition will be formed on the internal side walls of the reactor.
[0068] The reactors of the preferred embodiment I, II, and III are used for depositing a thin film on single substrate, so that they are not suitable for mass production. On the other hand, the following reactors of the preferred embodiment IV and V are suitable for mass production of the substrates with a thin film.
[0069] Please refer to FIG. 7, which shows a structural diagram of a HVPE reactor according to the preferred embodiment IV of the present invention. As shown in FIG. 7, the HVPE reactor includes a vertical tube 71 , a first gas heater 75 , a second gas heater 76 , a reaction chamber 77 , at least an input flow diaphragm 79 , and at least a gas exist slit 710 . The reaction chamber 77 includes a container space 78 . And, the substrates 73 for being deposited thereon are positioned at the bottom of the container space 78 .
[0070] The first gas heater 75 is positioned at the external side wall of the vertical tube 71 , and the second gas heater 76 is positioned on the external bottom of the vertical tube 71 . The reaction chamber 77 is located inside the vertical tube 71 and is a cylindrical reaction chamber. The input flow diaphragm 79 is positioned on the top of the reaction chamber 77 , and the at least a gas exist slit 710 is located on the internal side wall of the reaction chamber 77 with a particular distance from the substrates 73 . An extended diffusion layer 711 is formed from the height of the at least a gas exist slit 710 to the bottom of the reaction chamber 77 . The reaction chamber 77 is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrates 73 are sapphire substrates.
[0071] The HVPE reactor of the preferred embodiment IV is used for depositing the thin film 712 on each of the substrates 73 by reactions between the vertical input reagent gas flow 72 and the substrates 73 . And, an opposite-direction vertical output reagent gas flow 74 is produced after each reaction. The vertical input reagent gas flow 72 and the vertical output reagent gas flow 74 can be exhausted through the gas exist slit 710 .
[0072] The vertical input reagent gas flow 72 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 712 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 74 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases.
[0073] In the preferred embodiment IV, the substrates 73 are not directly reacted with the blowing of the vertical input reagent gas flow 72 . The reactions are proceeded during the diffusion process of the vertical input reagent gas flow 72 in the extended diffusion layer 711 . And, the vertical input reagent gas flow 72 is still in a gas state during the diffusion process. The second gas heater 76 is used for controlling the temperature difference between the substrates 73 and the internal side walls of the reactor, so that no deposition will be formed on the internal side walls of the reactor.
[0074] Please refer to FIG. 8, which shows a structural diagram of a HVPE reactor according to the preferred embodiment V of the present invention. As shown in FIG. 8, the HVPE reactor includes a vertical tube 81 , a plurality of first gas heaters 85 , a plurality of second gas heaters 86 , a plurality of reaction chambers 87 , at least an input flow diaphragm 89 , and at least a gas exist slit 810 . Each of the reaction chambers 87 includes a container space 88 . And, each of the substrates 83 for being deposited thereon is positioned at the bottom of each container space 88 .
[0075] The first gas heaters 85 are positioned on the external side walls of the vertical tubes 81 respectively, and the second gas heaters 86 are positioned at the external bottoms of the vertical tubes 81 . The reaction chambers 87 are respectively located inside the vertical tubes 81 and are cylindrical reaction chambers. The input flow diaphragm 89 is positioned on a top of the reaction chamber 87 , and the gas exist slit 810 is located on the internal side wall of the reaction chamber 87 with a particular distance from the height of the substrate 83 . A plurality of extended diffusion layers 811 are respectively formed from the gas exist slits 810 to the bottoms of the reaction chambers 87 . The reaction chambers 87 are made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrates 83 are sapphire substrates.
[0076] The HVPE reactor of the preferred embodiment V is used for respectively depositing the thin film 812 on the substrate 83 by a reaction between the vertical input reagent gas flow 82 and the substrate 83 . And, an opposite-direction vertical output reagent gas flow 84 is produced after the reaction. The vertical input reagent gas flow 82 and the vertical output reagent gas flow 84 can be exhausted through the gas exist slit 810 .
[0077] The vertical input reagent gas flow 82 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 812 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 84 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases.
[0078] In the preferred embodiment V, the substrate 83 is not directly reacted with the vertical input reagent gas flow 82 . The reaction is proceeded during the diffusion process of the vertical input reagent gas flow 82 in the extended diffusion layer 811 . And, the vertical input reagent gas flow 82 is still in a gas state during the diffusion process. The second gas heater 86 is used for controlling the temperature difference between the substrate 83 and the internal side walls of the reactor, so that no deposition will be formed on the internal side walls of the reactor.
[0079] The reactors of the preferred embodiment I, II, III, IV, and V are the main designs of the HVPE reactors in the present invention. The following reactor of the preferred embodiment VI is an extended reactor of the preferred embodiment I.
[0080] Please refer to FIG. 9, which shows a structural diagram of a HVPE reactor according to the preferred embodiment VI of the present invention. As shown in FIG. 9, the HVPE reactor includes a vertical tube 91 , a first gas heater 95 , a second gas heater 914 , a third gas heater 96 , a reaction chamber 97 , at least a second input flow diaphragm 99 , a plurality of first input flow diaphragms 912 , at least a gas exist slit 910 , a Ga vessel 913 , and a water cooled flange 915 . The reaction chamber 97 includes a container space 98 . And, the substrate 93 for being deposited thereon is positioned at the bottom of the container space 98 .
[0081] The first gas heater 95 is positioned on one external side wall of the vertical tube 91 , the second gas heater 914 is positioned on another external side wall of the vertical tube 91 , and the third gas heater 96 is positioned at the external bottom of the vertical tube 91 . The reaction chamber 97 is located inside the vertical tube 91 and is a cylindrical reaction chamber. The second input flow diaphragm 99 is positioned on the top of the reaction chamber 97 and upon the first input flow diaphragms 912 positioned inside the vertical tube 91 . The gas exist slit 910 is located on the internal side wall of the reaction chamber 97 with a particular distance from the substrate 93 . An extended diffusion layer 911 is formed from the height of the gas exist slit 910 to the bottom of the reaction chamber 97 . The reaction chamber 97 is made of a material selected from a group consisting of steel, quartz, sapphire, and ceramics. The substrate 93 is a sapphire substrate.
[0082] The HVPE reactor of the preferred embodiment VI is used for depositing the thin film 916 on the substrate 93 by a reaction between the vertical input reagent gas flow 92 and the substrate 93 . And, an opposite-direction vertical output reagent gas flow 94 is produced after the reaction. The vertical input reagent gas flow 92 and the vertical output reagent gas flow 94 can be exhausted through the gas exist slit 910 .
[0083] The vertical input reagent gas flow 92 is a mixture of HCl, GaCl, NH 3 , and Ar gases. The thin film 916 is a compound semiconductor selected from a group consisting of III-V groups and their alloys, IV group and their alloys, and GaN. The vertical output reagent gas flow 94 is a mixture of HCl, GaCl, NH 3 , Ar, and H 2 gases. The first input flow diaphragm 912 is for extending the flowing routes of the vertical input reagent gas flow 92 and the vertical output reagent gas flow 94 , and enhancing the thermal interaction between the reagent gas flow 92 and 94 . Furthermore, the volume of the reactor can be effectively reduced by the design of first input flow diaphragm 912 .
[0084] In the preferred embodiment VI, the substrate 93 is not directly reacted with the vertical input reagent gas flow 92 . The reaction is proceeded during the diffusion process of the vertical input reagent gas flow 92 in the extended diffusion layer 911 . And, the vertical input reagent gas flow 92 is still in a gas state during the diffusion process. The third gas heater 96 is used for controlling the temperature difference between the substrate 93 and the internal side walls of the reactor, so that no deposition will be formed on the internal side walls of the reactor.
[0085] As above-mentioned, the features of the HVPE reactors provided by the present invention include:
[0086] 1. The reactor has a design of a vertical input reagent gas flow and a vertical output reagent gas flow being oppositely directed and thermally coupled. The design makes the effect of the gas heating improved effectively and allows a reactor with a smaller volume. Besides, with the ability of quick responding to the changes of the temperature and the reagent gas flowing rate, the HVPE reactors are potentially suitable for the growth of quantum well structures.
[0087] 2. With the design of an extended diffusion layer, the input reagent gas flow can be reacted with the substrate in a gas state during the diffusion process, so that it is possible to enhance the utilization efficiency of the reagents and obtain a good growth uniformity of the thin film.
[0088] 3. The external bottom gas heater of the HVPE reactors according to the present invention allows the control of the temperature difference between the substrate and the internal side wall of the reactor, so that no deposition is formed on the internal side walls of the reactor.
[0089] 4. The reaction chamber of the present invention is a cylindrical chamber with high symmetry, so that it is easy to control the model the deposition processes.
[0090] Thus, the advantages of the HVPE reactors provided by the present invention can be summarized as follows:
[0091] 1. Good deposition uniformity.
[0092] 2. High efficiency of gas reagent utilization.
[0093] 3. Compact design.
[0094] 4. Easily controlling and modeling the deposition processes due to the high symmetry.
[0095] 5. Possibility of using low power heater.
[0096] 6. Possibility of growing a QW structure.
[0097] 7. Possibility of suppressing the deposition on the reactor walls.
[0098] While the invention has been described in terms of what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention needs not be limited to the disclosed embodiment. On the contrary, it is intended to cover various modifications and similar arrangements included within the spirit and scope of the appended claims which are to be accorded with the broadest interpretation so as to encompass all such modifications and similar structures. | A chemical vapor deposition reactor for depositing a thin film on at least a substrate through a reaction between a vertical input reagent gas flow and the at least a substrate is provided, in which a vertical output reagent gas flow is produced after the reaction. The reactor includes a vertical tube, at least a reaction chamber located inside the vertical tube, an input flow baffle located on the at least a reaction chamber, and at least a gas exit installed on the at least a reaction chamber for exhausting the vertical input reagent gas flow and the vertical output reagent gas flow. In addition, the substrate is located at the bottom of the at least a reaction chamber. The provided reactors allow the achievement of more efficient heating process, lower gas consumption and higher growth uniformity than the conventional reactors. | 2 |
The present invention comprises a rapidly-acting antimicrobial composition which is topically applied.
BACKGROUND OF THE INVENTION
Infection control and epidemiology experts have repeatedly emphasized that the single most important element in reducing the spread of infection is handwashing because a common method of transfer among individuals in the health care environment is with the hands. This fact has been painfully demonstrated in the analysis of epidemic spread.
However obvious and simple this may seem, medical care personnel, including physicians and nurses, are reluctant to wash or scrub their hands as frequently as required by their own protocols. It is estimated that the average time of washing between patients is 10 sec or less. The effectiveness of soap-and-water washing is measured in terms of minutes. Most simply do not wash frequently enough.
The product described herein is designed for repeated use by health care personnel when moving from patient to patient or procedure. The use of alcohol as an antimicrobial dates to biblical times and earlier. Its use was in vogue as a hand dip in the United States in the early years of this century, but it rapidly declined when new liquid soaps containing antimicrobials were introduced. A common complaint after the use of an alcohol dip was drying and chapping of the hands.
In Germany, Austria and Holland, alcohol has been widely accepted as an effective and useful hand rub and dip to the exclusion of most other types. The addition of emollients has eliminated some complaints relating to the natural action of alcohol as a defatting agent. Ethyl alcohol however does not defat in the same way that isopropyl alcohol act as a defatting agent.
Rotter in Austria has shown that a little-used alcohol, n-propyl or n-propanol is very effective, in fact, the most effective alcohol in reducing acquired microbial flora on the hands. When a health care worker handles equipment or patients, bacteria which are not a part of the normal skin flora are picked up and adhere loosely to the topmost skin layer, the stratum corneum.
It is the acquired and potentially pathogenic organisms that must be removed prior to handling another patient or medical device or before donning gloves. In recent years, serious outbreaks of infection and contamination in food and dairy plants have focused attention on handwashing by handlers of food and dairy products. Food, meat or dairy products provide a ready nutrient source for potentially pathogenic microorganisms acquired from natural sources or the handlers themselves.
SUMMARY OF THE INVENTION
It is the object of the present invention to provide an antimicrobial composition that is effective against a broad range of microorganisms, including pathogenic microorganisms that resist conventional antimicrobial compositions, that is easily applied as a topical composition, and that acts within seconds rather than minutes. Surprisingly, the present inventors have achieved this object with a composition comprising triclosan, chloroxylenol, and an alcohol or alcohol mixture.
DETAILED DESCRIPTION
More particularly, the present invention is a composition comprising from about 0.5 to about 3.0% by weight of triclosan, from about 0.5 to about 2.0% by weight of chloroxylenol, and from about 40 to about 70% by weight of an alcohol or alcohol mixture.
Alcohols--A variety of alcohols have been used in a multitude of concentrations. Isopropanol, although often used on the skin, is less desirable for use in the present invention because of its severe defatting tendency. Its defatting tendency may, however, be compensated for by adding sufficient emollient ingredient (as described herein). Preferred alcohols according to the present invention are ethyl and n-propyl. Ethyl alcohol has been the classic for medical application, but varies in effectiveness depending on the concentration and is regarded as the least effective relative to isopropyl and n-propyl. Normal propyl alcohol (n-propanol) has gained popularity in Austria and Germany because of its demonstrated effectiveness and from its use as a standard against which all other formulations are measured.
In the present invention, when more than one alcohol is used, the alcohols are mixed at a concentration that is peak for their activity. Ethyl alcohol is included for its reduced defatting activity and for activity against viruses, especially the lipophilic group. The inclusion of n-propanol enhances the contribution of alcohol to effectiveness.
A preferred mixture of alcohols is ethanol and n-propanol, each present in an amount of about 40 to about 70% by weight of the composition.
Antimicrobials
Triclosan--This relatively newer type of antimicrobial has a wide spectrum of antimicrobial action, including gram positive and gram negative bacteria. It is also a substantive antimicrobial and is currently incorporated into many cosmetic and drug-type cosmetic products used on the skin. Preferably, the concentrations used are low (in the 0.05 to 0.2 or 0.3% range). However, concentration can be increased to maximize the substantive action and enhance its immediate action.
Chloroxylenol (PCMX or parachlorometaxylenol)--This chemical has been used in products for skin application since 1933. It acts against a broad microbial spectrum, including gram negative organisms and fungi in particular. The concentration utilized in this formula is a preservative-effective amount and is included to inhibit contamination potential when the formulation is applied from multiple-use containers or from reservoirs frequently used in hospital settings.
Emollients--The emollient and humectant ingredients are optionally present to reduce the normal drying and defatting characteristics of alcohol. Preferred emollients are oil of mink and glycerin. Other emollient and/or humectant ingredients include silicone oil and aloe vera.
Surfactants--Surfactants are optionally included as emulsifiers and as a spreading agent in the formula. Preferred surfactants are Dow surfactant and Tween 20.
Perfuming Agents--Optionally, the present invention includes one or more perfuming agents. Preferred perfuming agents are vanilla extract and oil of peppermint. The scent of chloroxylenol is difficult to cover and vanillin is the most often used perfuming agent to cover it. The odor is clean but attractive. This characteristic is important since the majority of users are women.
Chelating Agents--One or more chelating agents are optionally included in the present antimicrobial formulations to enhance their activity against gram negative organisms, Pseudomonas in particular. Disodium edetate is a preferred chelating agent.
The antimicrobial compositions of the present invention can be administered with gimmicks, gadgets, sprays, foams, and attractive formulations that induce personnel to wash their hands. The present formulation can be used in attractive ways such as in a timed spray, an automated machine, a foam application or as a liquid hand rub. A small volume is used and it dries rapidly. A single washing procedure can be executed in 10-15 seconds, or the time routinely given to handwashing, rather than requiring minutes for effectiveness. No aerosols distributing microorganisms and/or microorganisms on skin particles into the air are produced in use. The agitation and friction resulting from the rubbing aids the effectiveness of alcohol. The vigorous rubbing over the hands when the product is used can be adapted to ensure that personnel cover all parts of the hand stressing those parts like the thumbs which are often missed in routine handwashing.
One detracting factor in the analysis of the handwashing practices in hospitals is the lack of convenient sinks for handwashing. An outstanding attribute of alcohol-based products is that no sink or water source is required. This is also an asset in emergency situations.
Another element that is desirable in analyzing the antimicrobial action of products on the skin is persistence, or substantivity of an antimicrobial agent, as dermatologists have termed it.
The definition of substantivity is the binding of a chemical to the dead skin cells of the stratum corneum (top-most layer of the skin). For an antimicrobial, activity is maintained so that bacteria in the hair follicles do not easily re-establish the skin microflora that has been removed. It is uncertain whether there is continued action on bacteria picked up as transient microflora from patient care or procedures, but it is probable that such organisms would not reproduce or establish themselves as resident microflora if this activity is present.
The formula described herein as unique and original combines many of the desirable attributes for a handwashing product for health care and can be applied to other areas where handwashing is becoming important.
The results show that this formula was more effective than a standard isopropanol/quaternary formula and the control, 60 percent isopropyl alcohol, when applied as a timed spray from an automated machine. There was greater than a 4-log 10 reduction of organisms artificially applied to the hands.
Minimal inhibitory concentrations of the formula when tested against a panel of organisms showed that the compounds included as active antimicrobials have a broad spectrum of activity.
The hands of personnel involved in the test showed no signs of irritation after the test or as a result of multiple uses in the laboratory.
Tests also showed that microorganisms did not contaminate or colonize the machine when it was operated many times a day (at least 100 time per day).
The present invention is described in greater detail with reference to the following examples, although it is in no way limited thereto.
EXAMPLE 1
A composition was prepared having the following ingredients:
______________________________________ Percent w/v______________________________________Irgasan DP-300 Triclosan 1.000Nipacide PX-PCMX 0.500Triton N-101 0.010Disodium Edetate 0.011Dow Surfactant 190 0.200Emulan Oil of Mink, light fraction 0.025Tween 20 0.800Glycerin, USP 1.000Imitation Vanilla Extract 0.040Oil of Peppermint, USP 0.00051-Propanol 39.550 v/vAlcohol SD40, Anhydrous 39.550 v/vDistilled Water, qs ad 100.000______________________________________
Physical Stability
Thirty-five ml were filled into capped 60 ml bottles made of clear glass, high density polyethylene, or high density polypropylene. Duplicate samples were wet down at 56 degrees C., ambient room temperature, and 50 degrees C. Samples were evaluated for changes in weight, color and clarity. Results are tabulated as follows.
______________________________________Percentage Change in Content WeightCondition Time Sample Glass HDPE HDPP______________________________________5C 4 mo A -0.13 -0.10 -0.06 B 0 -0.03 -0.10RT 10 mo A +0.29 -0.48 -0.19 B +0.16 -0.39 -0.2650C 6 mo A +0.06 -2.18 -1.20 B +0.19 -2.26 -1.56______________________________________Physical ObservationsCon- Containerdition Time Glass HDPE HDPP______________________________________5C 4 mo slight swirl white particles white particles at bottom present present colorless colorless colorlessRT 10 mo clear clear clear colorless colorless colorless50C 6 mo clear hazy clear very slight very slight very slight tan color tan color tan color______________________________________
EXAMPLE 2
Microbiological Testing of a Rapid Acting Formulation for Topical Administration
Introduction:
Rapid killing of microorganisms on skin is increasingly an important issue in the nosocomial transmission of infection in medical care facilities. Recent regulations from OSHA and recommendations from CDC have further sharpened the focus on hand washing and gloving in patient care. OSHA has issued regulations concerning the protection of Health Care Workers including requirements for implementation of infection control measures.
Objective:
It was discovered that the combination utilized in the present compositions exhibit unexpected synergism in terms of antimicrobial spectrum and speed of activity. The following studies were designed to show that the complete formulation of the present invention is more effective in rapid killing of high bacterial populations than any of its parts individually.
Materials:
A. Microbial Cultures:
1. Staphylococcus epidermidis ATCC 6538
2. Pseudomonas aeruginosa 15442
3. Salmonella choleraesuis ATCC 10708
4. Escherichia coli ATCC 11229
5. Candida albicans ATCC 10231
6. Serratia marcescens ATCC 14041
7. Group D streptococci Cl 012 (clinical isolate)
8. Streptococcus faecalis Cl 154 (clinical isolate)
9. Staphylococcus epidermidis ATCC 17917
10. Shigella species Cl 036 (clinical isolate).
B. Microbiological Media:
Trypticase Soy Broth (TSB)
Trypticase Soy Agar (TSA)
Phosphate Buffered Saline (PBS)
C. Miscellaneous Materials
Membrane filters
Filtration equipment
Spectrometer
D. Test Solutions
E. 0.5% chloroxylenol only--in the formulation ID No. 658
F. 1.0% triclosan only--in the formulation ID No. 659
G. 1.0% triclosan complete formulation ID No. 660 0.5% chloroxylenol
H. 40% n-propanol and 40% ethanol
I. 80% ethanol
J. 80% n-propanol
Test Procedure:
1. A 24 to 48 hr culture of each organism was standardized spectrophotometrically to provide a culture with a count of 10 9 -10 10 cfu/ml. The actual count was determined by dilution and plating on TSA.
2. One ml of the adjusted culture was added to 9 ml of PBS.
3. A sterile membrane was wet with 10 ml of PBS.
4. The tube of diluted culture was added to the wetted filter and filtered, leaving the bacteria on the face of the filter.
5. With the filtration was cut off, 3 ml of one of the test solutions was added to the inoculated filter.
6. After a 2-second exposure, diluent was poured onto the filter (at least 25 ml) and filtered immediately.
7. The filter was removed and placed onto the surface of a TSA plate. Incubation was at 35 ±2 degrees C.
8. The number of colonies recovered on the filter was counted after 48-hr incubation.
__________________________________________________________________________Comparative Results of Formulations Tested Formulation CodeOrganism Tested E F G H I J__________________________________________________________________________ Staphylococcus epidermidis TNTC 0 0 TNTC TNTC TNTC Pseudomonas aeruginosa TNTC TNTC TNTC TNTC TNTC TNTC Salmonella choleraesuis 3 0 0 6 15 3 Escherichia coli TNTC 0 0 TNTC 250 350 Candida albicans TNTC 300 0 TNTC 300 300 Serratia marcescens TNTC TNTC ˜400 TNTC TNTC TNTC Group D streptococci 0 0 0 0 0 0 Streptococcus faecalis 10 8 0 ˜300 31 35 Staphylococcus epidermidis 0 TNTC 0 TNTC TNTC TNTC10. Shigella species TNTC 250 0 TNTC TNTC TNTC__________________________________________________________________________ note: TNTC = too numerous to count.
The results of this test show that the complete formulation is more effective than any of its mixtures of components. This procedure for testing simulates application of the product to a surface such as skin. The exposure time in the test was extremely short, but in use hospital personnel frequently employ very short exposure times during patient care or in emergency situations.
Conclusions
1. The complete formulation was effective in the test system against a very high challenge counts of a wide variety of microorganisms in a very short period of time.
2. The effectiveness of the complete formulation was more effective than any of the mixtures of the ingredients in the formulation. | A rapidly-acting topically applied antimicrobial composition is disclosed which comprises triclosan, chloroxylenol, and an alcohol or alcohol mixture. | 0 |
BACKGROUND
[0001] The present invention relates generally to operations performed and equipment utilized in conjunction with a subterranean well and, in an embodiment described herein, more particularly provides diameter based tracking for a window milling system.
[0002] In a typical re-entry window milling system, a milling assembly including a lead mill and a follow (or watermelon) mill are deflected laterally relative to a casing or liner string by a milling whipstock. This lateral deflection causes the mills to cut through the casing string to thereby form a window in the casing sidewall. The mills may also be used to drill through cement and/or an earth formation surrounding the casing string, thereby starting a branch wellbore extending outward from the window.
[0003] Generally, the lead mill is used to initiate penetration of the casing sidewall, while the follow mill is used to enlarge the window and form it to the desired final shape and dimensions. For reduced resistance to penetration of the casing sidewall, the lead mill may have a smaller diameter than the follow mill, although the mills could have the same diameter. The whipstock deflects both of the mills using the same inclined surface, so that the mills displace along substantially the same path relative to the casing string.
[0004] Unfortunately, certain problems arise from use of such prior window milling systems. For example, large bending stresses are experienced when mills having different diameters are guided using the same deflection surface. As another example, substantial wear is experienced when both mills traverse the same surface during the milling operation. Furthermore, prior systems do not take advantage of the unique qualities of the different mills which could be made possible by guiding the mills along respective different paths.
[0005] Accordingly, it may be seen that improvements are needed in the art of window milling systems.
SUMMARY
[0006] In carrying out the principles of the present invention, a window cutting system and associated methods are provided which solve at least one problem in the art. One example is described below in which the system includes a whipstock or diverter which independently guides the different mills used to cut a window. Another example is described below in which multiple independent guide paths and wear surfaces are formed on the diverter, which is then installed in a well.
[0007] In one aspect of the invention, a window cutting system is provided which includes a cutting assembly with multiple cutting faces for cutting the window. A diverter is configured for guiding displacement of the cutting assembly relative to the window. The diverter includes multiple separate guide paths for the respective multiple cutting faces.
[0008] In another aspect of the invention, a method of cutting a window through a tubular string in a subterranean well includes the steps of: positioning a diverter in the tubular string, the diverter including multiple separate guide paths for respective multiple cutting faces of a cutting assembly; and then contacting the guide paths with the cutting faces to thereby form the window.
[0009] In yet another aspect of the invention, a method of cutting a window through a tubular string in a subterranean well includes the step of: positioning a diverter in the tubular string, the diverter including multiple separate guide paths for respective multiple cutting faces of a cutting assembly, and with each of the guide paths providing a separate wear surface for the respective cutting face.
[0010] These and other features, advantages, benefits and objects of the present invention will become apparent to one of ordinary skill in the art upon careful consideration of the detailed description of representative embodiments of the invention hereinbelow and the accompanying drawings, in which similar elements are indicated in the various figures using the same reference numbers.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 (Prior Art) is a partially cross-sectional view of a known window milling system;
[0012] FIG. 2 is an enlarged scale cross-sectional view of a diverter for use in a window cutting system embodying principles of the present invention;
[0013] FIG. 3 is an enlarged scale schematic cross-sectional view of the diverter, taken along line 3 - 3 of FIG. 2 ;
[0014] FIG. 4 is an elevational view of the diverter;
[0015] FIG. 5 is a schematic cross-sectional view of a first alternate configuration of the diverter;
[0016] FIG. 6 is a schematic cross-sectional view of a second alternate configuration of the diverter;
[0017] FIG. 7 is a schematic cross-sectional view of a third alternate configuration of the diverter;
[0018] FIG. 8 is an elevational view of a cutting assembly for use in the window cutting system;
[0019] FIG. 9 is an elevational view of a first alternate configuration of the cutting assembly; and
[0020] FIG. 10 is an elevational view of a second alternate configuration of the cutting assembly.
DETAILED DESCRIPTION
[0021] It is to be understood that the various embodiments of the present invention described herein may be utilized in various orientations, such as inclined, inverted, horizontal, vertical, etc., and in various configurations, without departing from the principles of the present invention. The embodiments are described merely as examples of useful applications of the principles of the invention, which is not limited to any specific details of these embodiments.
[0022] In the following description of the representative embodiments of the invention, directional terms, such as “above”, “below”, “upper”, “lower”, etc., are used for convenience in referring to the accompanying drawings. In general, “above”, “upper”, “upward” and similar terms refer to a direction toward the earth's surface along a wellbore, and “below”, “lower”, “downward” and similar terms refer to a direction away from the earth's surface along the wellbore.
[0023] Representatively illustrated in FIG. 1 is a prior art window milling system 10 . In the system 10 , a whipstock 12 is used to laterally deflect a milling assembly 14 , in order to mill a window 16 through a sidewall of a casing string 18 . The milling assembly 14 includes a lead mill 20 , a follow mill 22 and a tubular extension 24 which spaces apart the two mills.
[0024] As depicted in FIG. 1 , the lead mill 20 has partially traversed an inclined deflection surface 26 of the whipstock 12 , and has been thereby deflected laterally into contact with the casing string 18 . As a result, the lead mill 20 has penetrated the sidewall of the casing string 18 to initiate formation of the window 16 .
[0025] The follow mill 22 has also contacted the inclined surface 26 of the whipstock 12 , but has not yet contacted the casing string 18 . However, due to the larger diameter of the follow mill 22 , this contact between the follow mill and the surface 26 tends to raise the lead mill 20 off of the surface. The contact between the lead mill 20 and the casing string 18 tends to bias the lead mill toward the surface 26 .
[0026] Thus, it will be appreciated that an undesirable situation results from the use of a single surface 26 to guide the mills 20 , 22 toward the casing string 18 . Very large bending stresses are induced in the extension 24 due to the deflections of the lead mill 20 relative to the surface 26 when the follow mill 22 contacts the surface. The deflections of the lead mill 20 also cause an irregular, unstable milling of the window 16 . Furthermore, in traversing the surface 26 , both of the mills 20 , 22 cause wear of the same surface, thus requiring that the whipstock 12 be constructed of more expensive wear resistant materials, or that the whipstock be replaced during the milling operation (which is both time-consuming and expensive to accomplish) when the surface is excessively worn.
[0027] Referring additionally now to FIG. 2 , a cross-sectional view of a diverter 28 which embodies principles of the present invention is representatively illustrated. The diverter 28 may be used in place of the whipstock 12 in the system 10 described above.
[0028] However, it should be clearly understood that the diverter 28 could be used in other systems in keeping with the principles of the invention. For example, the diverter 28 could be used in window cutting systems in which windows are formed through any type of tubular string, such as liner strings, casing strings, tubing strings, etc. The diverter 28 could be used with window cutting assemblies which include any number, combination and configurations of mills, drills, cutting faces, etc. Thus, the uses of the diverter 28 , and the principles of the invention, are not limited in any manner to the details of the system 10 described herein.
[0029] One unique feature of the diverter 28 is that it provides multiple guide paths 30 , 32 for the respective multiple cutting faces of a cutting assembly. In the example depicted in FIG. 2 , the two guide paths 30 , 32 correspond to the respective lead mill 20 and follow mill 22 of the milling assembly 14 , although it will be appreciated that many other configurations are possible.
[0030] Another unique feature of the diverter 28 is that the guide paths 30 , 32 enable the mills 20 , 22 to be independently guided as they are displaced along the diverter. In turn, this provides the opportunity to utilize the mills 20 , 22 in ways not previously possible, for example, to form the window 16 in unique shapes, increase the stability of the mills during the cutting operation, increase the efficiency of the cutting operation, etc.
[0031] Yet another unique feature of the diverter 28 is that the guide paths 30 , 32 provide separate wear surfaces for the respective mills 20 , 22 . As described more fully below, the guide paths 30 , 32 may include intersecting portions at which the mills 20 , 22 traverse the same surface, but in the example depicted in FIG. 2 , the guide paths are at least in part independent of each other.
[0032] The paths 30 , 32 separately guide the mills 20 , 22 due to the difference in the diameters of the mills. In FIG. 3 , an enlarged scale lateral cross-sectional view of the diverter 28 is representatively illustrated, in which the difference in curvature of the guide paths 30 , 32 may be clearly seen.
[0033] The path 30 includes a surface 34 having concave curvature at radius r corresponding to the diameter of the lead mill 20 , whereas the path 32 includes a surface 36 having a concave curvature at a larger radius R corresponding to the larger diameter of the follow mill 22 . A result of this difference in curvature is that the lead mill 20 will contact and be guided by the surface 34 , while the follow mill 22 will contact and be guided by the surface 36 .
[0034] It is not necessary for the radius r to be exactly half of the diameter of the lead mill 20 , or for the radius R to be exactly half of the diameter of the follow mill 22 . For example, the radius r could be somewhat greater than the diameter of the lead mill 20 , but less than the diameter of the follow mill 22 , while the radius R could be somewhat greater than the diameter of the follow mill.
[0035] An elevational view of the diverter 28 is representatively illustrated in FIG. 4 . In this view the various surfaces which make up the guide paths 30 , 32 may be clearly seen.
[0036] The surfaces 34 , 38 , 40 , 42 have a relatively small curvature (corresponding to the smaller diameter of the lead mill 20 ) and are only contacted by the lead mill. The surfaces 36 , 44 , 46 , 48 have a relatively large curvature (corresponding to the larger diameter of the follow mill 22 ) and are only contacted by the follow mill. The surfaces 50 , 52 , 54 are designed to be contacted by both of the lead and follow mills 20 , 22 .
[0037] Thus, the guide path 30 for the lead mill 20 includes the surfaces 34 , 38 , 50 , 40 , 42 , 52 , 54 , and the lead mill will traverse these surfaces in that order. The guide path 32 for the follow mill 22 includes the surfaces 44 , 46 , 36 , 50 , 48 , 52 , 54 , and the follow mill will traverse these surfaces in that order. Note that the guide paths 30 , 32 intersect at the surfaces 50 , 52 , 54 .
[0038] In one unique feature of the guide paths 30 , 32 as configured in FIG. 4 , the lead mill 20 contacts and is deflected laterally outward by the surface 38 at the same time that the follow mill 22 contacts and is deflected laterally outward by the surface 46 . In this manner, both of the mills 20 , 22 are laterally supported by the diverter 28 when they contact and cut through the casing string 18 . This lateral support is also provided by the diverter 28 for both of the mills 20 , 22 when they are traversing the respective surfaces 40 , 36 which are not laterally inclined and do not deflect the mills outward.
[0039] It may now be more fully appreciated how the use of different guide paths enables enhanced shaping of windows. For example, the lead mill 20 may be deflected laterally at a different point along the diverter 28 as compared to the lateral deflection of the follow mill 22 . As another example, one of the mills 20 , 22 may traverse a surface which is not laterally inclined at a point on the diverter 28 where the other mill traverses a surface which is laterally inclined (e.g., the surface 38 traversed by the lead mill is laterally inclined at a point longitudinally along the diverter where the surface 36 traversed by the follow mill is not laterally inclined).
[0040] This ability to independently deflect and guide the cutting faces of the mills 20 , 22 opens up a wide variety of possibilities for creating uniquely shaped windows. Furthermore, the multiple guide paths 30 , 32 provide increased support to the mills 20 , 22 during the cutting operation (for example, the lead mill 20 can be supported by the guide path 32 while the follow mill 22 simultaneously contacts and is guided by the path 30 ), which reduces bending stresses in the extension 24 , and the multiple guide paths can increase the stability of the mills during the cutting operation. These features are of substantial benefit especially when both of the mills 20 , 22 are cutting through the casing string 18 , and also when only the lead mill is cutting through the casing string.
[0041] Referring additionally now to FIG. 5 , a schematic cross-sectional view of a longitudinal portion of an alternate configuration of the diverter 28 is representatively illustrated. In this view it may be seen that the guide path 32 includes an undulating surface 56 . For example, the surface 56 may have a sinusoidal shape with a period of length L.
[0042] Preferably, the period L of the surface 56 is less than the length of an outer cutting face 58 of the follow mill 22 . In this manner, the cuts made by the cutting face 58 will overlap along the length of the window 16 , producing a substantially constant width of the window. However, it is not necessary for the surface 56 to be shaped so that the cuts made by the cutting face 58 overlap, since in some circumstances it may be desired to produce windows with other than constant widths.
[0043] One benefit of using the undulating surface 56 in the guide path 32 is that it produces a lateral oscillating (in-and-out) displacement of the follow mill 22 relative to the casing string 18 as the follow mill traverses the surface. It is known that when the centerline of the follow mill 22 is inline with the sidewall of the casing string 18 , an unstable situation results. The oscillating motion of the follow mill 22 produced by the surface 56 permits the follow mill to displace back and forth through the sidewall of the casing string 18 , cutting a width of the window 16 at least as great as the diameter of the follow mill along a substantial length of the window, without the follow mill centerline having to remain inline with the sidewall of the casing string for any substantial amount of time.
[0044] In addition, note that the guide path 30 as depicted in FIG. 5 does not include a surface which also produces a similar oscillating motion of the lead mill 20 . This is due to the fact that the guide paths 30 , 32 are independent of each other. However, it should be understood that the guide path 30 could include a surface which produces an oscillating motion of the lead mill 20 in keeping with the principles of the invention.
[0045] Referring additionally now to FIG. 6 , a schematic elevational view of a longitudinal portion of another alternate configuration of the diverter 28 is representatively illustrated. In this view it may be seen that the guide path 32 includes an undulating surface 60 . For example, the surface 60 may have a sinusoidal shape with a period of length L.
[0046] The surface 60 is similar to the surface 56 described above, except that it produces a lateral oscillating motion of the follow mill 22 which is orthogonal to that produced by the surface 56 . In other words, the surface 56 produces an in-and-out motion of the follow mill 22 relative to the sidewall of the casing string 18 , whereas the surface 60 produces a side-to-side motion of the follow mill relative to the casing string sidewall.
[0047] The surface 60 may have a sinusoidal shape with a period of length L which, similar to the surface 56 as described above, produces an overlapping of the cuts generated by the cutting face 58 . In this manner, the width of the window 16 can be greater than the diameter of the follow mill 22 , even where the centerline of the follow mill is not inline with the sidewall of the casing string 18 . It will be appreciated by those skilled in the art that this is a substantial benefit in the art of window milling, at least in part because access and flow through the window 16 is enhanced by the increased width, and a smaller diameter mill may be used for a given window width (thereby reducing the torque required to drive the mill and increasing the efficiency of the cutting operation).
[0048] However, it should be understood that it is not necessary for the cuts made by the follow mill 22 to overlap in the manner described above. For example, it may be desirable in some situations for the cuts to not overlap, or to only partially overlap, to thereby produce other desired shapes of the window 16 .
[0049] In addition, note that the guide path 30 as depicted in FIG. 6 does not include a surface which also produces a similar side-to-side oscillating motion of the lead mill 20 . This is due to the fact that the guide paths 30 , 32 are independent of each other. However, it should be understood that the guide path 30 could include a surface which produces an oscillating motion of the lead mill 20 in keeping with the principles of the invention.
[0050] It may be desirable to combine the displacements produced by the surfaces 56 , 60 described above. For example, the guide path 32 could include a surface which is helically formed and thereby produces both an in-and-out and side-to-side motion of the follow mill 22 as it traverses the surface. The guide path 30 could include such a surface for producing a similar motion of the lead mill 20 , as well.
[0051] An alternate configuration of the diverter 28 as depicted in FIG. 7 demonstrates one manner in which the guide path 30 can include a surface 62 which produces an oscillating displacement of the lead mill 20 . In this example, the surface 62 has a sinusoidal shape with a period of length L which is less than the length of an outer cutting face 64 of the lead mill 20 . This configuration enables the lead mill 20 to cut through the sidewall of the casing string 18 and produce an initial opening which has a greater width than the diameter of the lead mill.
[0052] It will be appreciated that the guide path 30 can also be configured with surfaces which produce a side-to-side motion of the lead mill 20 , a combination of in-and-out and side-to-side motions, or any other type or combination of displacements. In addition, the guide paths 30 , 32 may produce any displacements of the mills 20 , 22 separately and independently of each other. This enables any desired shape of the window 16 to be formed, and allows the unique capabilities of each of the mills 20 , 22 to be utilized to their greatest extent, among other benefits.
[0053] Referring additionally now to FIG. 8 , an elevational view of a cutting assembly 66 which embodies principles of the present invention is representatively illustrated. The cutting assembly 66 may be used in place of the milling assembly 14 in the system 10 described above.
[0054] However, it should be clearly understood that the cutting assembly 66 could be used in other systems in keeping with the principles of the invention. For example, the cutting assembly 66 could be used in window cutting systems in which windows are formed through any type of tubular string, such as liner strings, casing strings, tubing strings, etc. The cutting assembly 66 could be used with any whipstocks or diverters which include any number, combination and configurations of surfaces, etc. Thus, the uses of the cutting assembly 66 , and the principles of the invention, are not limited in any manner to the details of the system 10 described herein.
[0055] As depicted in FIG. 8 , the cutting assembly 66 is a one-piece structure which includes a lead mill 68 , a follow mill 76 and an extension 72 which spaces apart the two mills. The lead mill 68 includes an outer cutting face 74 which has a smaller diameter than an outer cutting face 76 of the follow mill 70 . A bore (not visible in FIG. 8 ) extends longitudinally through the cutting assembly 66 .
[0056] Note that the lead mill 68 includes multiple angled blades. Each blade is symmetric and includes multiple faces, one of which is parallel with the longitudinal axis of the lead mill 68 .
[0057] The follow mill 76 also includes multiple angled blades, each of which has multiple faces, one of which is perpendicular to the longitudinal axis of the follow mill. A trailing face of the follow mill 76 has a concave generally frusto-conical profile and has a smaller diameter than that of the lead mill 68 .
[0058] The one-piece construction of the cutting assembly 66 provides a very rigid structure which is also very strong due to the absence of threads, etc. joining the various components of the assembly to each other. However, it should be understood that cutting assemblies utilizing separately formed components may be used in keeping with the principles of the invention.
[0059] An alternate configuration of the cutting assembly 66 is representatively illustrated in FIG. 9 . In this configuration, the follow mill 70 includes an inclined or tapered leading cutting face 78 . In addition, the lead mill 68 includes a leading inclined cutting face 80 and the cutting face 74 is also inclined.
[0060] The lead mill 68 includes multiple angled blades. Each blade is symmetric and includes multiple faces, all of which are inclined relative to the longitudinal axis of the lead mill 68 . The leading cutting face 80 is inclined to match the angle of the surface 42 of the diverter 28 .
[0061] The follow mill 76 also includes multiple angled blades, each of which has multiple faces, all of which are inclined relative to the longitudinal axis of the follow mill. The leading cutting face 78 is inclined to match the angle of the surface 38 of the diverter 28 . Thus, when the cutting faces 80 , 78 simultaneously traverse the respective surfaces 42 , 38 of the diverter 28 , the cutting assembly 66 is displaced laterally outward, while the longitudinal axis of the cutting assembly remains parallel to the longitudinal axis of the diverter.
[0062] Therefore, it will be appreciated that any configuration of the cutting assembly 66 may be used in keeping with the principles of the invention. For example, any number, placement, type and combinations of cutting faces may be used, any of the cutting faces (e.g., the leading face) on the lead mill 68 and/or follow mill 70 may include blades, cutters, etc.
[0063] As yet another example, depicted in FIG. 10 is another alternate configuration of the cutting assembly 66 , schematically illustrated in a cross-sectional view. In this configuration, the respective cutting faces 74 , 76 of lead and follow mills 68 , 70 are made up of an array of individual cutting teeth or elements 82 , such as carbide “buttons.”
[0064] In addition, an end surface 84 of the lead mill 68 and an outer surface 86 of the extension 72 are covered with a cutting material. A suitable cutting material for use on the surfaces 84 , 86 is known as CUTRITE™, and is available from Halliburton Energy Services, Inc. of Houston, Tex., USA.
[0065] The use of the cutting material on the surfaces 84 , 86 allows the sidewall of the casing string 18 to be cut by portions of the cutting assembly 66 other than the lead and follow mills 68 , 70 . Indeed, since substantially all of the lower portion of the cutting assembly 66 is capable of cutting the sidewall of the casing string 18 , it may be considered that the lead and follow mills 68 , 70 are not really separate components of the cutting assembly or separate “mills”—instead, the cutting assembly may be considered as being made up of multiple cutting faces. These multiple cutting faces may be independently guided by a whipstock or diverter, as described above.
[0066] In a method which incorporates principles of the invention, a window (such as the window 16 ) is cut through a tubular string (such as the casing string 18 ) in a subterranean well. A diverter (such as the diverter 28 ) is positioned in the tubular string. When so positioned, the diverter includes multiple separate guide paths (such as the guide paths 30 , 32 ) for respective multiple cutting faces (such as the cutting faces 74 , 76 ) of a cutting assembly (such as the cutting assembly 66 ). Then, the guide paths are contacted by the cutting faces to thereby form the window. The guide paths are able to independently guide the cutting faces to form the window.
[0067] Of course, a person skilled in the art would, upon a careful consideration of the above description of representative embodiments of the invention, readily appreciate that many modifications, additions, substitutions, deletions, and other changes may be made to these specific embodiments, and such changes are within the scope of the principles of the present invention. Accordingly, the foregoing detailed description is to be clearly understood as being given by way of illustration and example only, the spirit and scope of the present invention being limited solely by the appended claims and their equivalents. | Diameter based tracking for a window milling system. A window cutting system includes a cutting assembly with multiple cutting faces for cutting the window; and a diverter for guiding displacement of the cutting assembly relative to the window, the diverter including multiple separate guide paths for the respective multiple cutting faces. A method of cutting a window includes the steps of: positioning a diverter in a tubular string, the diverter including multiple separate guide paths for respective multiple cutting faces of a cutting assembly; and then contacting the guide paths with the cutting faces to thereby form the window. Another method of cutting a window includes the step of: positioning a diverter in the tubular string, the diverter including multiple separate guide paths for respective multiple cutting faces of a cutting assembly, with each of the guide paths providing a separate wear surface for the respective cutting face. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
The present application is a continuation application of U.S. application Ser. No. 10/689,873 entitled “System And Method for Remote Passenger and Baggage Check-In.” It also claims priority to U.S. Provisional Application 60/420,042 entitled “Remote Passenger and Baggage Check-In Method and System” filed on Oct. 21, 2002, and incorporated herein in its entirety by reference.
FIELD OF THE INVENTION
The present invention relates generally to common carrier baggage processing. More particularly, the present invention relates to a system and method for remote baggage check-in.
BACKGROUND OF THE INVENTION
Checking in baggage and obtaining a boarding pass for travel via common carriers (e.g., commercial air or cruise line) can be inconvenient and time-consuming. The time required for checking baggage and obtaining a boarding pass has been made even more cumbersome after added security measures adopted following the terrorist airplane hijackings of Sep. 11, 2001. A need exists to provide the traveling public with improved services that permit convenient and secure interim baggage storage, remote passenger and baggage check-in, and timely transfer of baggage from a remote property to a common carrier point of departure.
Services are known in the art for advance pickup of passenger baggage from a remote property and direct delivery to an airport for check-in. However, such prior services typically require long lead times, such as for example, up to 12 to 24 hours, before airline departure time, permitting baggage screening during off-peak periods. In addition, boarding passes are not issued in advance.
Prior attempts have been made to improve remote baggage processing. For example, Certified Airline Passenger Services (CAPS) of Las Vegas, Nev., attempted to provide remote passenger and baggage processing from 1998 until 2001. CAPS used hotels as a point of remote baggage check-in, providing a third party check-in counter in hotel lobbies. The CAPS service was not integrated into hotel operations. Instead, these check-in counters and related staff members were made available to hotel guests as a clearly separate service being offered by a third party other than the hotel. Hotel guests could check their baggage and pick up boarding passes at a hotel lobby station, thus avoiding both activities at the airport.
The CAPS approach suffered from several limitations and eventually the company was unable economically to continue its service. For example, the CAPS approach used CAPS employees whose sole function was baggage and passenger processing. Such staffing proved costly. Employees were occupied for only limited times (when customers were checking bags) but needed to be available for long periods of time (whenever customers might request the service) and the service would only be used by passengers if the fee charged were minimal (e.g., $6.00 per passenger). Some economies of scale could be achieved at mega-hotels (e.g., 4000+ rooms), but the number of such hotels are limited and larger hotels require more employees to support times when many guests want to check bags at the same time.
Another example of an attempt to improve common carrier baggage processing systems is described in U.S. Pat. No. 6,512,964 entitled Baggage Transportation System and listing Quackenbush, et al. as inventors. The Quackenbush patent describes using the Internet to capture travel information from a user including an origin location and a destination location. The baggage is collected from the origin location, taken to an origin airport where it placed on a correct flight, and delivered from a destination airport to the destination location.
The Quackenbush patent fails to provide important teachings that may ultimately determine the viability of the service when implemented, if ever. The Quackenbush patent indicates that a Ground Delivery Operator (GDO) picks up baggage from an origin location and takes it to an origin airport. However, there is no teaching of how customers check in baggage. It is not clear if the passenger has to wait for a GDO to travel to where the customer is or, if a GDO is located at the remote property, how staffing issues are addressed. Indeed, there is nothing in the Quackenbush patent that helps solve the staffing problems faced by known remote baggage processing systems, such as the CAPS service.
Thus, there is a need for an improved common carrier passenger and baggage processing system. Further, there is a need for a remote common carrier passenger and baggage processing system that cross-utilizes employees at the remote property. Even further, there is a need for baggage and passenger check-in kiosks for such remotely located common carrier passenger and baggage processing systems.
SUMMARY OF THE INVENTION
The present invention is directed to a system and method for delivering integrated services for remote passenger baggage handling and check-in. In an exemplary embodiment, these services are implemented by fully integrating with existing operations and staff at remote properties. In this way, remote baggage check-in and boarding pass issuance may be handled in the course of guest departures at the remote property. The integration with existing operations can be accomplished through the use of an outsourcing arrangement between a remote baggage check-in service provider and the remote properties.
For a fee, the service provider supplies and manages trained and FAA approved staff for bellhop, valet, and parking garage positions (collectively, “attendants”) at the remote property. In addition to their customary roles, the attendants handle remote baggage check-in, baggage temporary storage, boarding pass issuance, and secure transportation of baggage from the remote property to common carriers' points of departure. The system and method provide passengers with a seamless and transparent interface to remote baggage check-in services. Economic and operational advantages derive from using the same integrated staff for remote property and remote baggage check-in services. High labor costs inherent in the use of separate and dedicated staff to provide similar services are avoided.
Since the same attendant performs the traditional bellhop, valet, or parking garage duties, as well as the remote baggage check-in services, the cost burden of the remote baggage handling inactivity is substantially subsidized. Thus, greater work capacity is provided during peak periods of guest departures at the remote properties. At the same time, the incremental operating cost for such services over the conventional operating costs for bellhop, valet and parking garage attendants is quite small.
Briefly, one exemplary embodiment relates to a method for remotely arranging the transportation of baggage for passengers of a common carrier. The method includes receiving travel information for a passenger via a communications network, identifying passenger baggage to be transported, and cross-utilizing employees of a remote property to obtain possession of the identified passenger baggage and manage transportation of the passenger baggage from the remote property to a common carrier origin identified in the received travel information.
Another exemplary embodiment relates to a computer-based baggage transportation system. The system includes a server computer, a client computer, and an attendant. The server computer includes travel information for a plurality of common carriers. The client computer is coupled via a network to the server computer and is configured to check in baggage and passengers from a property that is remote from a common carrier departure location. The attendant is cross-utilized with the remote property. That is, the attendant performs remote common carrier check-in services as well as remote property services. The attendant has met federal agency approval standards for common carrier check-in services.
Yet another exemplary embodiment relates to a method in a remote baggage and passenger check-in system. The method includes obtaining passenger identification information for a passenger, using the passenger identification information to retrieve travel information for the passenger from a server computer, printing a boarding pass for the passenger based on the retrieved travel information, printing a baggage identification label for passenger baggage at a property remote from a common carrier departure location, transferring possession of the passenger baggage from the passenger to an attendant at the remote property, securely transporting the passenger baggage from the remote property to the common carrier departure location, and transferring possession of the passenger baggage to the common carrier. The attendant at the remote property has remote property responsibilities and baggage management responsibilities and the attendant is qualified to obtain possession of the passenger baggage.
Other principle features and advantages of the invention will become apparent to those skilled in the art upon review of the following drawings, the detailed description, and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Exemplary embodiments will hereafter be described with reference to the accompanying drawings.
FIG. 1 is a flow diagram depicting operations in a remote baggage and passenger processing system in accordance with an exemplary embodiment.
FIG. 2 is a flow diagram depicting operations in a secured baggage transport system in accordance with an exemplary embodiment.
FIG. 3 is a diagrammatic representation of the inter-relationships between a service provider, one or more remote properties, and one or more common carrier points of departure.
FIG. 4 is a diagrammatic representation of a remote baggage and passenger processing system in accordance with an exemplary embodiment.
FIG. 5 is a user interface for a workstation used in the remote baggage and passenger processing system of FIG. 4 .
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
FIG. 1 illustrates operations performed in an exemplary embodiment of a remote baggage and passenger processing system. Additional, fewer, or different operations can be performed in alternative embodiments. A remote intake process takes place at a remote property 81 ( FIG. 3 ), such as a hotel, office, resort, or convention center. A guest 84 arrives (block 20 ) at the remote property 81 . An attendant 83 determines an airline 82 with which the guest has a reservation (block 22 ). The attendant 82 asks the guest 84 for her ticket, as well as at least one form of government-issued identification, such as a driver's license or U.S. passport (block 23 ).
The attendant 83 may accept remote baggage check-in any time prior to the pre-departure cutoff time, which may vary according to the traffic conditions, locations of remote properties and common carrier 82 points of departure and weather conditions. The cut-off time is selected to ensure timely delivery of baggage to the airlines with sufficient time before flight time to process and load the baggage onto the plane. Such cut-off times can be two to four hours before a common carrier departure time. Thus, the attendant 82 must confirm the guest flight departure time and final destination (blocks 24 , 25 ).
Using industry-standard common use terminal equipment (CUTE), the attendant 83 confirms the guest's 84 reservation (block 26 ). The attendant 83 matches the guest, her identification and reservation-information (block 27 ). If the attendant 83 determines there is a match, the attendant prints a boarding pass (block 28 ), affixes one or more baggage claim tickets to the ticket folder, and inserts the boarding pass into the ticket folder, returning the completed ticket folder to the guest (block 29 ). The attendant 83 attaches identification tags or labels to the baggage. The attendant 83 charges the guest 84 for the remote baggage check-in service according to a standardized pricing schedule, making the receipt available to the guest 84 .
The attendant 83 stores the guest's baggage 85 in an FAA and airline approved storage room at the remote property 81 , which is secured against unauthorized entry (block 32 ). The attendant 83 places the baggage 85 in an airline-specific location within the room (block 33 ). As part of the storing operation, the attendant 83 scans the baggage 85 , which has been tagged using a bar code or other similar means for uniquely identifying each piece of baggage. The attendant 83 scans the tag to digitally record a unique identifying code for each piece of baggage 85 (block 34 ). Finally, the attendant 83 secures and exits the storage room, and returns to his station in the remote property 81 to receive the next guest 84 .
FIG. 2 is a flow chart of a secured baggage transport process of an exemplary embodiment. Additional, fewer, or different operations can be performed in alternative embodiments. One or more attendants 63 from each remote property 81 may be designated as a driver, who periodically transports baggage to the common carrier via securable truck 86 . At a scheduled interval, the driver prepares for baggage transfer and enters the storage room at the remote property 51 (blocks 50 , 51 ). The driver loads baggage onto the truck via wheeled carts designated for each common carrier 82 , tagging baggage 85 bound for the earliest departure time for that transfer run (blocks 52 , 53 ). The driver completes the baggage loading while performing a scanner inventory of each piece of baggage 85 (block 54 ). The driver locks the truck storage compartment using a tamper-proof seal, coded with a unique identifying number (block 55 ). Alternatively, the carts can be securely sealed with the tamper-proof seal instead of the truck, or both the carts and the truck can be sealed. The driver records the unique identifying number of the tamper-proof seal (on the truck or on the carts) and calls to notify the airlines of the truck departure and other pertinent information (block 56 , 57 ). The driver transports the sealed truck containing the baggage to the airport (block 58 ) and delivers the baggage 85 to each airline 82 . Finally, the driver returns to the remote property to begin the cycle again (block 60 ).
FIG. 3 illustrates a diagram depicting exemplary interrelationships between the service provider 80 , one or more remote properties 81 , and one or more common carrier 82 points of departure. The service provider's attendants 83 are integrated into operations of a remote property. The service provider 80 can furnish attendants 83 to the remote properties through an outsourcing arrangement. For example, in the case of a hotel remote property, these attendants, as employees or agents of the service provider, work as members of the hotel staff, in the capacity of bellhop, valet, security, or parking garage attendant. In these roles, attendants 83 can immediately provide guests 84 with remote baggage check-in services without the need to redirect the guest to a specialized and separate location at the remote property 81 .
At pre-determined time intervals, an attendant (driver) at each remote property 81 retrieves baggage 85 from the secured storage room at the remote property 81 , loads and transfers the baggage 85 via securable truck 86 to the common carrier 82 , and delivers individual pieces of baggage 85 to the appropriate airline or other common carrier 82 .
FIG. 4 illustrates a diagram depicting a remote baggage and passenger processing system 100 having a baggage and passenger processing server 102 coupled to a network 104 . The network 104 can be a virtual private network (VPN) providing communication access between the server 102 and a kiosk 106 and/or an employee workstation 108 . The kiosk 106 is a small structure having a display and an electronic processor located nearby or within the remote property where a passenger can provide identification, such as a credit card, and interact with the server 102 to check-in, receive a boarding pass, and check any baggage the passenger may have. The kiosk 106 has a printing device that prints a boarding pass for the passenger as well as baggage claim tickets. An attendant finalizes the baggage check-in process by obtaining an identification label for the baggage, attaching it, and taking possession of the baggage. In an exemplary embodiment, an attendant printer separate from the kiosk 106 is used for the printing of baggage identification labels or stickers.
The employee workstation 108 is a computer dedicated to processing baggage and passengers and operated by an attendant. A person of skill in the art will appreciate that the employee workstation 108 could be coupled to other networks, such as the Internet, but that concerns for security of the server 102 and the travel information available within the server 102 may justify limiting the employee workstation 108 to only a dedicated network, such as the network 104 . The employee workstation 108 includes a computer and printer and performs the same check-in operations as the kiosk 106 .
When a customer uses the kiosk 106 for checking in baggage, a service provider attendant or employee at the remote property can perform a verification of the identification of the individual passenger. Further, the attendant takes and labels the passenger baggage with identification tags or stickers. These tags may have bar coding on them to facilitate tracking of the baggage. The attendant takes possession of the baggage for secure storage and delivery of the baggage to the common carrier, as described above with reference to FIGS. 1-3 .
FIG. 5 illustrates an example user interface 120 for a workstation used in the remote baggage and passenger processing system 100 described with reference to FIG. 4 . The user interface 120 provides for the location of flight reservations according to flight information (e.g., flight number, departure or arrival city), frequent flyer number, passenger name record, or a record number. A selection of how to search for a flight can be made by selecting an option in portion 122 of the user interface 120 .
A portion 124 of the user interface 120 provides a graphical host interface where flight information is displayed and passenger and baggage check-in information can be entered. The interface depicted in portion 124 connects a workstation at a remote property with a server containing common carrier information. Other user interfaces can be utilized, including interfaces for different devices. For example, a user interface for a kiosk may include drop down menus, text boxes, and other features to simplify interaction with the passenger.
Advantageously, the user interface 120 provides one unified graphical user interface for all airlines or common carriers. As such, attendants can service passengers for many different carriers instead of just one. The user interface 120 can also include information regarding passenger and baggage check-in requirements that trains (or reminds) attendants to specific common carrier baggage and passenger rules and requirements. For example, different airlines (or other common carriers) may have different weight restrictions for checked baggage or restrictions on the number of bags per passenger. The user interface 120 informs the attendant of such common carrier specific requirements such that applicable action can be taken, such as a surcharge for heavy baggage or additional bags beyond a per passenger limit.
The remote baggage and passenger processing system and method described with reference to FIGS. 1-5 provide an economically feasible solution to the time-consuming and cumbersome task of checking baggage at a common carrier. One advantage to the cross-utilization of employees at a remote property is the ability for the service to financially withstand shut-downs. If, for example, airlines cancel flights for a period of time, attendants continue to do remote property functions, even though the baggage and passenger processing services are unavailable.
This detailed description outlines exemplary embodiments of a remote baggage and passenger processing system and method. In the foregoing description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the present invention. It is evident, however, to one skilled in the art that the exemplary embodiments may be practiced without these specific details. In other instances, structures and devices are shown in block diagram form in order to facilitate description of the exemplary embodiments.
While the exemplary embodiments illustrated in the Figures and described above are presently preferred, it should be understood that these embodiments are offered by way of example only. Other embodiments may include, for example, a wide range of technological tools used by employees at the remote property, including wireless handheld devices, barcode printing devices, and many other different technologies. The invention is not limited to a particular embodiment, but extends to various modifications, combinations, and permutations that nevertheless fall within the scope and spirit of the appended claims. | A computer-based baggage transportation system includes a client computer and an attendant. The client computer is coupled via a network to a server computer and is configured to check in baggage and passengers from a property that is remote from a common carrier departure location. The attendant is cross-utilized with the remote property. That is, the attendant performs remote common carrier check-in services as well as remote property services. The attendant has met federal agency approval standards for common carrier check-in services. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a divisional of U.S. patent application Ser. No. 09/543,288 filed Apr. 5, 2000 now U.S. Pat. No. 6,585,769 which claims the benefit of U.S. Provisional Patent Application No. 60/127,735, filed Apr. 5, 1999, the entire disclosure of which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
The present disclosure relates generally to prosthetic members for joining or repairing bone segments, including artificial ligaments and, more specifically, to an artificial ligament intended for partial or full replacement of the anterior longitudinal ligament of the anterior lumbar, thoracic or cervical spine.
Ligaments extend between adjacent bone structures and serve a primary function of maintaining and providing appropriate stability to the bone structures to maintain the structures in aligned, spaced relation, particularly when subjected to loads in tension or upon torsional movement. Spinal ligaments stabilize and support vertebral bodies during movement of the spine.
During surgical treatment of the spine, a section of a spinal ligament may be resected to provide access to a diseased or damaged intervertebral disc and/or to permit introduction of a fusion implant, bone graft or intervertebral disc prosthesis intended for long term support of the vertebral bodies. The bone graft, fusion implant or intervertebral disc return stability to the spinal column in compression and flexing, however, due to removal of the spinal ligament, the biomechanical characteristics of extension and torsional stability lost by the ligament's removal must be replaced. Current techniques involve the use of metal bone plates which are secured to the vertebral bodies with screw locking mechanisms. Conventional bone plates, however, are rigid and, thus, significantly inhibit spine mobility. Additionally, the screw locking mechanisms utilized with such plates are relatively complicated and provide minimal flexibility with respect to fastener positioning, etc.
SUMMARY OF THE INVENTION
Accordingly, the present disclosure is directed to a simple and flexible artificial ligament which easily conforms to a patient's anatomy and can be used independently or in combination with an intervertebral graft, implant or prosthesis. In one preferred embodiment, an artificial spinal ligament is in the form of a flexible conformable plate dimensioned to span adjacent vertebrae and having openings for reception of bone screws, fasteners, etc. to mount the plate to the vertebrae. The biomechanical supporting characteristics of the plate approximate the characteristics of the ligament (e.g., anterior spinal) which it replaces thereby providing appropriate support to the spine in extension which also permitting normal spine mobility. A method of supporting adjacent vertebrae with the artificial ligament is also disclosed.
BRIEF DESCRIPTION OF THE DRAWINGS
Preferred embodiments of the disclosure are described herein with reference to the drawings wherein:
FIG. 1 is a perspective view of the artificial ligament of the present disclosure;
FIG. 2 is a top plan view of the artificial ligament of FIG. 1 ;
FIG. 3 is a cross-sectional view taken along lines 3 — 3 of FIG. 2 ;
FIG. 4 is a perspective view of an alternate embodiment illustrating mounting thereof to the vertebral column;
FIG. 5 is a top plan view of an alternate embodiment of FIG. I;
FIG. 6 is a cross-sectional view taken along lines 6 — 6 of FIG. 5 ; and
FIG. 7 is a perspective view of another alternate embodiment of the artificial ligament.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring now to the drawings, in which like reference numerals identify similar or identical elements throughout the several views, there is illustrated the artificial ligament of the present disclosure. The artificial ligament of the present disclosure is intended to replace part or all of the supporting function of a ligament previously removed in connection with a surgical procedure. The artificial ligament has particular application in replacing the supportive function of a spinal ligament, e.g., anterior or posterior, which may have been fully or partially resected during a spinal procedure. The artificial ligament is advantageously dimensioned to be positioned to span adjacent vertebrae to restore the natural biomechanics, e.g., including tensional support and range of motion, of the removed ligament segment. The artificial ligament is contemplated for use with a bone graft, fusion implant or artificial disc to compliment the compressive load characteristics of the implant with its tensional supporting capabilities during healing. It is also envisioned that the ligament may be utilized in other capacities such as, for example, repair of other body ligaments such as the anterior crucial ligament, etc.
Referring initially to FIGS. 1–3 , artificial ligament 100 includes ligament body or plate 102 which is advantageously dimensioned to span at least two adjacent vertebrae. It is envisioned that the ligament body 102 may span three or more vertebral bodies. In a preferred embodiment, the length “l” of ligament body 102 ranges from about 1–3 inches, preferably about 2 inches.
Ligament body 102 is preferably fabricated from a generally flexible material. The selected flexible material of ligament body 102 preferably has physical characteristics which approximate the biomechanical characteristics of the spinal ligament which it replaces. More specifically, the selected material of ligament body 102 supports the spine and provides stability in extension, i.e., the ligament body has tensional load bearing capabilities while also permitting a degree of flexibility approximating the natural ligament. A preferred material of fabrication for ligament body 102 includes a flexible polymeric material such as polyethylene.
Ligament body 102 defines first and second web body end portions 104 connected through intermediate body portion 106 . Web body end portions 104 each include a pair of apertures 108 for reception of bone fasteners 110 . As best depicted in FIG. 2 , apertures 108 may be generally elongated or slotted in the longitudinal direction with respect to longitudinal axis “a” of body 102 to permit multi-position capabilities of the bone fasteners 110 with respect. to ligament body 102 and the vertebral bodies as will be discussed. Apertures 108 are preferably countersunk defining a beveled or chamfered surface 112 adjacent the upper surface of the ligament body 102 for reception of the head 114 of the bone fasteners 110 in flush relation therewith. Although two apertures 108 are shown in each web end portion 104 of the preferred embodiment, it is envisioned that each web portion 104 may have more than two apertures or only one aperture. With particular reference to FIG. 2 , intermediate body portion 106 has a width “w” which is substantially less than the corresponding width of web portion 104 . Such dimensioning reduces the transverse profile of ligament body 102 thereby increasing flexibility to facilitate torsional movement of ligament body 102 upon corresponding movement of the patient's spine. The width “w” of intermediate body portion 102 ranges from about 0.125 inches to about 0.375 inches, more preferably, about 0.250 inches.
With reference again to FIG. 1 , bone fasteners 110 serve as anchoring means for securing the ligament body 102 to the adjacent vertebrae. The preferred bone fastener 110 includes a fastener head 114 and a fastener shaft 116 extending from the fastener head. The fastener shaft 116 is threaded preferably with a self-tapping thread 118 . Upon mounting of bone fastener 110 within the adjacent vertebrae, the fastener head 114 is preferably flush with the upper surface of the ligament body 102 . Other anchoring means for mounting ligament body 102 to the vertebral bodies are envisioned by one skilled in the art including expandable bolts, screws, non-threaded fasteners, etc.
In use in connection with an anterior spinal procedure, the anterior ligament is removed to permit access to a diseased or damaged disc section. A partial or full discectomy may be performed followed by insertion of a bone graft, fusion implant (e.g., as disclosed in U.S. Pat. No. 4,961,740, the contents of which are incorporated herein by reference) or an intervertebral prosthesis (such as disclosed in commonly assigned application Ser. No. 09/098,606, filed Jun. 17, 1998, the contents of which are incorporated herein by reference).
When used with fusion devices, the bone fasteners 110 are placed at the outer area 108 r of the openings 108 so the ligament is rigid in tension while allowing for compression. This provides for immediate stability in extension as extension loads immediately place the ligament in tension. The fasteners 110 are free to move within openings 108 relative to the ligament 102 in compression. This also permits graft compression.
When used with artificial discs, the fasteners 110 are placed in the middle 108 m or inner part 108 i of the openings 108 to permit limited relative motion of fasteners 110 within openings 108 of the ligament in both flexion and extension. Extension ultimately leads to tension in the ligament as the fasteners 110 meet the ends 108 r of the openings 108 . Thus, movement in tension and compression is provided. This flexibility also reduces the likelihood of the fasteners 110 backing out over time.
FIG. 4 illustrates an alternate embodiment of the artificial ligament where intermediate body portion 106 includes an elongated longitudinal depression 120 defining a reduced thickness of ligament body 102 . This reduced thickness permits the surgeon to create an additional opening 108 in the ligament body 102 to receive a bone fastener 110 for further fixation to the vertebrae. More specifically, during the surgical procedure the surgeon may create an opening at a desired location within intermediate body portion 106 with a punch or the like. A multitude of openings (shown in phantom) may be formed within depression 120 . This feature facilitates use of ligament body 102 in spanning more than two vertebrae, e.g., three vertebrae. FIG. 4 illustrates this embodiment mounted to the spinal column and spanning three (3) vertebral portions “v 1 –v 3 ” with the middle opening 108 having a fastener for attachment to the intermediate vertebrae “v 2 ” and the outer openings 108 having fasteners 110 mounted to respective vertebrae “v 1 ” “v 3 ”. Depression 120 preferably also defines a transverse dimension “t” which approximates the diameter of the fastener head 114 to facilitate retention of the head with respect to the ligament body 102 .
FIGS. 5 and 6 illustrate an alternate embodiment of the artificial ligament 100 of FIG. 1 . Artificial ligament 200 is substantially similar to the ligament 100 , but, differs primarily in its dimensioning. More specifically, the length “l” of ligament body 102 is shorter than the length “l” of the embodiment of FIG. 1 , preferably ranging in length from about 0.75–1.25 inches, more preferably about 1.14 inches. In all other respects, the ligament 200 is identical to ligament 100 Of FIG. 1 .
FIG. 7 illustrates another alternate embodiment of the ligament of the present disclosure. Ligament 300 includes a slight arcuate bend 302 or bump adjacent its intermediate portion. The arcuate bend provides a degree of excess material to permit the effective length of the ligament to increase when ligament 300 is placed in tensioned, i.e., the arcuate bend will tend to straighten under extension. The ligament 300 will become increasingly stiffer with a higher tension load. Multiple bends are also envisioned to establish non-linear stiffness.
While the above description contains many specifics, these specifics should not be construed as limitations on the scope of the disclosure, but merely as exemplifications of preferred embodiments thereof. For example, the present prosthetic device disclosed herein may be implanted to repair a variety of bone structures such as the ankle, knee, wrist, etc. Those skilled in the art will envision many other possible variations that are within the scope and spirit of the disclosure. | A method of repairing a bone joint by using a simple and flexible artificial ligament which easily conforms to a patient's anatomy and can be used independently or in combination with an intervertebral graft, implant or prosthesis to return stability to the spine subsequent to a surgical spine procedure, is disclosed. The method includes anchoring the artificial ligament to at least two vertebrae to aid in restoring stability to the compromised joint. The artificial ligament is also disclosed. | 0 |
CROSS REFERENCE TO RELATED APPLICATIONS
Reference is made to commonly assigned co-pending patent applications Ser. No. 10/431,066 filed herewith entitled “METHOD FOR FIELD PROGRAMMABLE RADIO FREQUENCY DOCUMENT IDENTIFICATION DEVICES” in the names of Anand V. Chhatpar, Jeffrey D. Pierce, Brian M. Romansky, Thomas J. Foth and Andrei Obrea; Ser. No. 10/430,911 filed herewith entitled “METHOD FOR FIELD PROGRAMMING RADIO FREQUENCY IDENTIFICATION DEVICES THAT CONTROL REMOTE CONTROL DEVICES” in the names of Jeffrey D. Pierce, Brian M. Romansky, Thomas J. Foth and Anand V. Chhatpar; Ser. No. 10/430,925 filed herewith entitled “METHOD FOR FIELD PROGRAMMABLE RADIO FREQUENCY IDENTIFICATION TESTING DEVICES FOR TRANSMITTING USER SELECTED DATA” in the names of Thomas J. Foth, Brian M. Romansky, Jeffrey D. Pierce, Andrei Obrea and Anand V. Chhatpar; Ser. No. 10/430,922 filed herewith entitled “METHOD FOR FIELD PROGRAMMABLE RADIO FREQUENCY IDENTIFICATION DEVICES TO PERFORM SWITCHING FUNCTIONS” in the names of Andrei Obrea, Brian M. Romansky, Thomas J. Foth, Jeffrey D. Pierce and Anand V. Chhatpar; Ser. No. 10/431,067 filed herewith entitled “METHOD FOR FIELD PROGRAMMING RADIO FREQUENCY IDENTIFICATION RETURN FORMS” in the names of Jeffrey D. Pierce, Thomas J. Foth, Brian M. Romansky, Andrei Obrea, and Anand V. Chhatpar; and Ser. No. 10/430,597 filed herewith entitled “METHOD AND APPARATUS FOR FIELD PROGRAMMING RADIO FREQUENCY IDENTIFICATION DEVICES” in the names of Brian M. Romansky, Thomas J. Foth, Jeffrey D. Pierce, Andrei Obrea and Anand V. Chhatpar.
This Application claims the benefit of the filing date of U.S. Provisional Application No. 60/419,361 filed Oct. 18, 2002, which is owned by the assignee of the present Application.
FIELD OF THE INVENTION
This invention pertains to electronic circuits and, more particularly, to programmable radio frequency product labels.
BACKGROUND OF THE INVENTION
Dangerous goods are substances and articles that are potentially hazardous to people and property. They may be corrosive, flammable, explosive, oxidizing or reactive with water, toxic, radioactive, etc. Whatever their properties and their potential for injury and destruction, great care is needed in their handling, storage and transport. Examples of dangerous goods are explosives, gun powder, blasting material, bombs, detonators, smokeless powder, radioactive materials, ammunition, atomic weapons, chemical compounds or any mechanical mixture containing any oxidizing and combustible units, or other ingredients in such proportions, quantities, or packing that ignite by fire, friction, concussion, percussion or detonation of any part thereof which may and is intended to cause an explosion; poisons; carcinogenic materials; caustic chemicals; hallucinogenic substances; illegal materials; drugs that are illegal to sell and/or dispense; and substances which, because of their toxicity, magnification or concentration within biological chains, present a threat to biological life when exposed to the environment, etc. All other types of goods may be considered normal goods.
The government has promulgated regulations regarding the storage, handling and shipment of dangerous goods. These Regulations are designed to prevent accidents, provide safety standards to protect workers, the community and the environment from the effects of fires, explosions and escapes of these dangerous goods.
Dangerous goods and normal goods may be shipped and stored in individual containers that may be placed in larger containers. The contents and descriptions of the goods and information pertaining to the goods in the individual containers and the contents and descriptions of the goods and information pertaining to the goods in the larger containers may be written directly on the containers and/or labels that are attached to the containers. One of the problems of the prior art was that the only way to determine the information written on the individual containers that are placed in larger containers was to remove the individual containers from the larger containers. The foregoing process is labor intensive, time consuming and expensive.
Another problem experienced by the prior art was that the information written on the containers and/or labels had to be directly scanned by optical scanners or directly viewed by humans in order to be read. An additional problem encountered by the prior art was that if many individual containers having goods were placed in a larger sealed container, someone may remove, i.e., steal some of the individual containers from the larger container and reseal the larger container without the custodian of the larger container realizing that some individual containers are missing.
Another problem of the prior art is that someone may remove an individual container from a larger sealed container and replace the removed container with a different container and then reseal the larger container without the custodian of the larger container realizing the change. This may result in a theft or dangerous goods being substituted for normal goods.
The information written on the containers and/or the information written on the labels that are attached to the containers may be written on paper and then entered into a computer. Typically, the information written on paper and/or labels is entered into computers by optically scanning the paper and/or labels. The foregoing method of entering information into computers is inconvenient, because the paper and/or label must be placed directly on the scanner, and no intervening objects may be placed between the paper and the scanner. Another method utilized by the prior art for writing information on paper and/or labels and entering the written information into a computer involved placing a piece of paper over an expensive digitizing pad and using a special pen that produced digital data by indicating the coordinates of the digitizing pad. Thus, heretofore, there was no economic, convenient way for wirelessly entering information written on plain paper, labels, and/or on containers into a computer.
Another method utilized by the prior art for entering information into a computer involved the use of radio frequency identification (RFID) tags. The RFID tags were programmed to contain digital information either during the manufacturing of the read only memory portion of the RFID integrated circuit, or in the field using electromagnetic radio frequency signals to store information in the nonvolatile memory portion of the RFID tag. One of the difficulties involved in the utilization of RFID tags was that if an end user wanted to enter information into the RFID tag, the end user had to use a specialized device that communicated with the RFID tag through a radio frequency. Another problem involved in the utilization of RFID tags that were programmed by the manufacturer was that the end user had to share the information that was going to be programmed into the RFID tag with the manufacturer of the tag.
SUMMARY OF THE INVENTION
This invention overcomes the disadvantages of the prior art by providing a method that allows one to mark information with a pencil on a material, equipped with a RFID type circuit, and have the marked information provided to the RFID circuit, or have the written information cause the RFID circuit to perform some function. The material may be any cellulose type product, i.e., paper, cardboard, chipboard, wood or plastic, fabric, animal hide, etc. The marked entered information may be corrected by erasing the written information, with an pencil eraser and writing new information on the paper or other material with a pencil. Information may also be marked into a RFID circuit or have the marked information cause the RFID circuit to perform some function by utilizing a standard ink jet computer printer to print lines on paper equipped with a RFID type circuit, by having the printed lines perform the function of wires. The aforementioned printed information may be modified by having an individual connect different printed wires by drawing a penciled line between the wires or by punching holes in the printed lines.
This invention accomplishes the foregoing by utilizing the RFID serial number generation portion of the RFID circuit that is used when the RFID circuit is being read. In the prior art, the bits used to encode one's and zero's into the generation portion of the RFID circuit were typically fixed. This invention utilizes the serial number generation portion of the RFID circuit by exposing on a piece of paper some or all of the bits left open or closed to represent a binary values, i.e., ones or zeros. A user may complete the RFID serial number storage portion of the RFID circuit by filling in the space between the connections with a pencil to alter the binary values. Alternatively, the serial number generation portion of the RFID circuit may be exposed on a piece of paper with all of the connections made, and a user may break a space between the connections with a sharp instrument or hole punch to alter the binary values. Alternatively, the serial number generation portion of the RFID circuit may have some of the bits all ready left open or closed to represent a unique number.
An additional advantage of this invention is that the one may be able to read the information written on individual containers and/or labels that are affixed to individual containers that are placed inside larger containers without opening the larger containers.
A further advantage of this invention is that when individual containers having goods were placed in a larger sealed container, someone will be able to determine that some of the individual containers have been removed from the larger container without opening the larger container.
A further advantage of this invention is that a custodian will be able to detect if someone removes an individual container from a larger sealed container and replaces the removed container with a different container and then reseal the larger container.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a prior art RFID circuit;
FIG. 2A is a drawing of a circuit 24 that replaces memory array 21 of FIG. 1 showing how programming of the bits may be accomplished by making the bits externally available for programming RFID circuit 10 ;
FIG. 2B is a drawing of a circuit 300 that is an alternate representation of circuit 24 , that replaces memory array 21 of FIG. 1 showing how programming of the bits may be accomplished by making the bits externally available for programming RFID circuit 10 ;
FIG. 3 is a drawing showing sensor circuit 25 of FIG. 2A in greater detail;
FIG. 4 is a drawing of a label to be completed by a party possessing dangerous goods that is going to be attached to a container;
FIG. 5 is a drawing of a label to be completed by a party having custody of goods that is going to be attached to a container; and
FIG. 6 is a drawing showing how a modified RFID circuit attached to a piece of paper may be altered to indicate a desired selection.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings in detail, and more particularly to FIG. 1 , the reference character 10 represents a prior art RFID circuit. Circuit 10 may be the model MCRF 200 manufactured by Microchip Technology, Inc. of 2355 West Chandler Blvd, Chandler, Ariz. 85224. RFID reader 11 is connected to coil 12 , and 12 is coupled to coil 13 . Coil 13 is connected to modulation circuit 14 . Modulation circuit 14 is connected to clock generator 15 and rectifier 16 . Modulation control 17 is coupled to modulation circuit 14 , clock generator 15 and counter 18 . Counter 18 is coupled to column decode 20 . Row decode 19 is coupled to memory array 21 , and array 21 is coupled to modulation control 17 . It would be obvious to one skilled in the art that a battery may be used to supply power to circuit 10 .
Reader 11 has a transmitter mode and a receiver mode. During the transmit mode of reader 11 , reader 11 transmits a radio frequency signal for a burst of time via coil 12 . After the transmission of a signal by reader 11 , reader 11 turns into a receiver. Coil 12 is inductively linked with coil 13 , and coil 13 receives the radio frequency signal from coil 12 and converts the aforementioned signal into inductive energy, i.e., electricity. When coil 13 has sufficient energy, coil 13 will cause clock generator 15 to generate timing pulses which drive counter 18 . Counter 18 drives row decode 19 which causes memory array 21 to read the fixed bit data pattern stored in memory array 21 one bit at a time. As the data bits are being read by array 21 , the data bits are transmitted to modulation control circuit 17 . Control circuit 17 sends the data bits to reader 11 via modulation circuit 14 and coils 13 and 12 .
FIG. 2A is a drawing of a circuit 24 that replaces memory array 21 of FIG. 1 showing how programming of the bits may be accomplished by making the bits externally available for programming RFID circuit 10 . A plurality of sensor circuits 25 is contained in circuit 24 . Sensor circuits 25 are labeled SC 1 SC 2 SC 3 . . . SC n . Line 29 is connected to SC 1 and graphite contact 52 and line 30 is connected to SC 2 and graphite contact 53 . Line 31 is connected to SC 3 and graphite contact 54 and line 32 are connected to SC n and graphite contact 55 . There is a sensor circuit 25 for each graphite contact. The description of FIG. 4 will describe how information may be entered into circuit 24 via graphite contacts 52 - 55 . SC 1 has an input 33 , which enables the data output 34 . Input 33 is connected to one of the n lines 37 , and data output 34 is connected to data line 36 and pull up resistor 35 . Data line 36 is connected to modulation control 17 (FIG. 1 ).
When counter 18 selects the value 1 , column decode 20 will enable line 33 , which will cause the same logic level that is on graphite contact 52 to be placed on data output 34 . When line 33 is not selected, the value on graphite contact 52 does not have any influence on the data output line 34 . Enable outputs 33 for SC 1 . . . SC n are bundled together in lines 37 so that only one line 37 is turned on at a time. Lines 37 are connected to column decode 20 . Column decode 20 is connected to counter 18 , and counter 18 is connected to row decode 19 . Counter 18 generates a sequence of numbers from 1 through n to enable a different line 37 in sequential order. Thus, data line 36 will receive the data outputs 34 from SC 1 . . . SC n at different times.
FIG. 2B is a drawing of a circuit 300 that is an alternate representation of circuit 24 , that replaces memory array 21 of FIG. 1 showing how programming of the bits may be accomplished by making the bits externally available for programming RFID circuit 10 . Circuit 300 includes AND gates 301 , 302 , 303 and 304 and OR gate 305 .
One of the inputs of AND gate 301 is connected to column decode 20 and the other input to AND gate 301 is connected to one of the ends of resistor 322 , one of the ends of diode 306 and one of the ends of diode 314 . The other end of resistor 322 is connected to ground. The other end of diode 306 is connected to one of the terminals of toggle switch 310 , and the other end of toggle switch 310 is connected to row decode 19 . The other end of diode 314 is connected to one of the terminals of toggle switch 318 , and the other end of toggle switch 318 is connected to row decode 19 .
One of the inputs of AND gate 302 is connected to column decode 20 , and the other input to AND gate 302 is connected to one of the ends of resistor 323 , one of the ends of diode 307 and one of the ends of diode 315 . The other end of resistor 323 is connected to ground. The other end of diode 307 is connected to one of the terminals of toggle switch 311 , and the other end of toggle switch 311 is connected to row decode 19 . The other end of diode 315 is connected to one of the terminals of toggle switch 319 , and the other end of toggle switch 319 is connected to row decode 19 .
One of the inputs of AND gate 303 is connected to column decode 20 , and the other input to AND gate 303 is connected to one of the ends of resistor 324 , one of the ends of diode 308 and one of the ends of diode 316 . The other end of resistor 324 is connected to ground. The other end of diode 308 is connected to one of the terminals of toggle switch 312 , and the other end of toggle switch 312 is connected to row decode 19 . The other end of diode 316 is connected to one of the terminals of toggle switch 320 , and the other end of toggle switch 320 is connected to row decode 19 .
One of the inputs of AND gate 304 is connected to column decode 20 , and the other input to AND gate 304 is connected to one of the ends of resistor 325 , one of the ends of diode 309 and one of the ends of diode 317 . The other end of resistor 325 is connected to ground. The other end of diode 309 is connected to one of the terminals of toggle switch 313 , and the other end of toggle switch 312 is connected to row decode 19 . The other end of diode 317 is connected to one of the terminals of toggle switch 321 , and the other end of toggle switch 321 is connected to row decode 19 .
Column decode 20 and row decode 19 function by taking the selected output at logic one, i.e., a high level and keeping all the other outputs at logic zero, i.e., a low level. The output of AND gates 301 - 304 are connected to the input of OR gate 305 , and the output of OR gate 305 is data that is connected to the input of modulation circuit 17 . If switches 310 , 311 , 312 and 313 , respectively, remain open, AND gates 301 - 304 , respectively, will have a “zero” output. If switches 310 , 311 , 312 and 313 , respectively, are closed, AND gates 301 - 304 , respectively, will have a “one” output. The output of AND gates 301 - 304 , respectively, will be read when switches 318 - 321 , respectively, are closed.
FIG. 3 is a drawing showing sensor circuit 25 of FIG. 2A in greater detail. The negative input of comparator 41 is connected to line 29 , and the positive input of comparator 41 is connected to line 38 . Comparator 41 may be a LM339N comparator. One end of line 38 is connected to a 2-3 volt reference voltage, and the other end of line 38 is connected to one of the ends of resistor 39 . The other end of resistor 39 is connected to the positive input of comparator 41 and one of the ends of resistor 40 . The other end of resistor 40 is connected to the input of NAND gate 42 , the output of comparator 41 and one of the ends of resistor 43 . The other end of resistor 43 is connected to a source voltage to act as a pull up resistor. The other input to NAND gate 42 is enable output 33 . The output of gate 42 is data output 34 . Resistor 39 may be 47,000 ohms, and resistor 40 may be 470,000 ohms. Resistor 43 may be 1,000 ohms. Comparator 41 has a positive feedback to provide a small amount of hysteresis
Sensor circuit 25 is a differential circuit that accommodates variations in the conductivity of the conductive material. The conductive material may be used as a voltage divider to produce V ref on line 38 under the same conditions experienced by paper in on line 29 . Thereby, nullifying the effects of varying resistance in the conductive material. It will be obvious to one skilled in the art that sensor circuit 25 may replace switches 310 - 313 and 318 - 321 of FIG. 2 B.
FIG. 4 is a drawing of a label to be completed by a party possessing dangerous goods that is going to be attached to a container. RFID circuit 10 is attached to material 100 by means of a conductive adhesive such as an anisotropic adhesive (not shown). The manufacturer, shipper and/or custodian of Dangerous goods may place the identity of the goods 98 , i.e., nitric acid and manufacturer information and/or other information 99 on material 100 by writing the identity 98 and information 99 on material 100 in a manner that identity 98 and information 99 may be, read by a RFID reader. Graphite contacts 101 - 107 and lines 108 - 114 are printed on material 100 with a standard computer printer, like the model Desk Jet 880C printer manufactured by Hewlett Packard using a Hewlett Packard 45 black ink cartridge.
If the custodian of a container having nitric acid to which material 100 is affixed or is going to be affixed decides that the nitric acid is toxic, the custodian uses a graphite pencil, i.e., number 2 , HB, etc., or a Paper Mate® black ball point pen to fill in rectangle 116 . If the custodian of a container having nitric acid to which material 100 is affixed or is going to be affixed decides that the nitric acid is corrosive, the custodian uses a graphite pencil, i.e., number 2 , HB, etc., or a Paper Mate® black ball point pen to fill in rectangle 118 . If the custodian of a container having nitric acid to which material 100 is affixed or is going to be affixed decides that the nitric acid loses its potency, expires and/or should only remain in the container until December 2004, the custodian uses a graphite pencil, i.e., number 2 , HB, etc., or a Paper Mate® black ball point pen to fill in rectangle 120 .
If the custodian of the container having nitric acid decides that the nitric acid is radioactive the custodian fills in rectangle 115 with a graphite pencil. If the nitric is flammable rectangle 117 is filled in with a graphite pencil and if the nitric acid loses its potency, expires and/or should only remain in the container until December 2004 rectangle 120 is filled in with a graphite pencil.
Hence, printed lines 108 - 114 perform the function of wires so that information may be modified in the RFID type circuit by having an individual connect different printed wires by drawing a penciled line between the wires, i.e., filling in rectangles 115 - 120 with a graphite pencil or by punching holes in rectangles 115 - 120 to supply information regarding the dangerous goods.
If the custodian of the container having nitric acid changes his/her mind regarding the classification of the goods or makes a mistake in filling in one of the rectangles, the custodian could erase the penciled marking in the rectangle with a pencil eraser so that a RFID reader would only read what the custodian indicated on material 100 . The custodian would affix material 100 to the nitric acid individual container (not shown), and the custodian would be able to read the completed material 100 even if material 100 and its container is placed in a larger container, without opening the larger container.
FIG. 5 is a drawing of a label to be completed by a party having custody of goods that is going to be attached to a container. RFID circuit 10 is attached to material 97 by means of a conductive adhesive such as an anisotropic adhesive (not shown). The manufacturer, shipper and/or custodian of goods, i.e. ABC Company may place the information regarding the goods 96 , on material 97 by writing information 96 on material 97 in a manner that information 96 may be, read by a RFID reader. Graphite contacts 121 - 124 and lines 135 - 148 are printed on material 97 with a standard computer printer, like the model Desk Jet 880C printer manufactured by Hewlett Packard using a Hewlett Packard 45 black ink cartridge.
If the custodian of a container having goods to which material 97 is affixed or is going to be affixed or is placed in the container containing the goods decides that the goods are containers of 325 mg aspirin that have 500 tablets in each container, the custodian uses a graphite pencil, i.e., number 2 , HB, etc., or a Paper Mate® black ball point pen to fill in rectangles 149 , 152 and 153 .
Hence, printed lines 135 - 148 perform the function of wires so that information may be modified in the RFID type circuit by having an individual connect different printed wires by drawing a penciled line between the wires, i.e., filling in rectangles 149 - 161 with a graphite pencil or by punching holes in rectangles 149 - 161 to supply information regarding the goods.
If the custodian of the container having aspirin changes his/her mind regarding the classification of the goods or makes a mistake in filling in one of the rectangles, the custodian could erase the penciled marking in the rectangle with a pencil eraser so that a RFID reader would only read what the custodian indicated on material 97 . For instance, if a model 1 calculated made in 2002 is in the container rectangles 156 and 158 would be filled in with a graphite pencil, i.e., number 2 , HB, etc., or a Paper Mate® black ball point pen. The custodian would affix material 97 to the individual container of aspirin (not shown) or place material 97 in the individual containers, and the custodian would be able to read the completed material 97 even if material 97 and its container is placed in a larger container, without opening the larger container. Thus, it will be easier to inventory the goods that are in the containers.
FIG. 6 is a drawing showing how a modified RFID circuit attached to a piece of paper may be altered to indicate a desired selection. RFID circuit 10 is attached to paper 231 by means of an adhesive (not shown). Graphite contacts 232 , 233 , 234 and 235 and lines 236 , 237 , 238 and 239 are printed on paper 231 by a standard computer printer like the model Desk Jet 880C printer manufactured by Hewlett Packard using a Hewlett Packard 45 black ink cartridge. If a human user wanted to alter the information represented by line 236 or 238 , the user would remove adhesive labels 241 or 242 on lines 236 or 238 . A RFID reader (not shown) will be able to read the above selection.
The above specification describes a new and improved label and RFID type circuit that uses printed lines to perform the function of wires so that information may be modified in the RFID type circuit by having an individual connect different printed wires by drawing a penciled line between the wires or by creating openings in the printed lines to supply information regarding the goods. It is realized that the above description may indicate to those skilled in the art additional ways in which the principles of this invention may be used without departing from the spirit. Therefore, it is intended that this invention be limited only by the scope of the appended claims. | A system and method that allows one to mark information with a pencil on a label equipped with a RFID type circuit, and have the marked information provided to the RFID circuit, or have the written information cause the RFID circuit to supply information regarding the goods that are contained in a individual container. Individual containers may be placed in a larger container. The marked entered information may be corrected by erasing the written information with a pencil eraser and writing new information on the paper with a pencil. Information may also be marked into a RFID circuit or have the marked information cause the RFID circuit to perform some function by utilizing a standard ink jet computer printer to print lines on paper equipped with a RFID type circuit, by having the printed lines perform the function of wires. The aforementioned printed information may be modified by having an individual connect different printed wires by drawing a penciled line between the wires or by punching holes in the printed lines. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a device for protecting gauge glasses.
2. Description of the Prior Art
It is customary to determine the level of water in a steam boiler by means of an external liquid level glass gauge assembly. Such an assembly typically comprises a thick walled transparent tube held in position by an upper and lower valve body arrangement. The upper valve body is connected to that portion of the boiler which is permanently in the vapor state and the lower valve body is connected to that portion of the boiler which should always contain water. Accordingly, the level of liquid in the transparent tube indicates the level of the vapor/liquid interface inside the boiler.
The criteria for the use and maintenance of such sight gauges are well known and are set forth in the suggested Rules of Care of Power Boilers (1971 Edition) (Section VII, Sub Section C2 201 through 210 and C5 608 through C5 609 published by The American Society of Engineers, New York, N.Y.). Because of the high pressures and temperatures involved in steam boilers it is desirable to have a tight seal between the gauge glass and the gauge glass holding bodies. This seal is usually provided by means of a rubber gasket which is compressed into place by a sealing nut. It has been found in practice that under operative conditions it is virtually impossible to maintain an absolutely leak-proof seal due to the degradation of the gasket material under operating conditions. Unfortunately, it is impractical to replace the gasket as soon as degradation begins. Therefore, it is the usual practice to put up with a certain amount of degradation in order to avoid the expense and inconvenience of shuting down the boiler at inopertune moments. If the gasket deteriorates while the boiler is operating at a high temperature and high pressure, then three serious disadvantages arise. First, the leaking vapor in aerosol form settles onto the sight gauge and obscures the line of vision, thereby preventing accurate readings. Second, the continual presence of such liquids will eventually erode the surface of the gauge glass. Thirdly, as the liquids evaporate they leave behind previously dissolved solid materials. It has been found that unless these deposits of solid materials are either prevented or are immediately removed, they will eventually cloud up the entire sight gauge. It is often difficult and unsafe to keep sight gauges clean since the gauges are generally located at a height of about 14 ft. above ground floor level and in very close proximity to boilers operating at temperatures in the range of 400° F.
The nature of this problem has been known for a good many years. One method for coping with the problem is to provide better sealing gaskets at both ends of the sight gauge. Devices for improving the sealing between both ends of the gauge glasses are discussed in U.S. Pat. Nos. 1,038,642 and 2,629,262. Alternatively, mechanisms have been proposed and used to help keep the gauges clean. One such solution is found in U.S. Pat. No. 1,234,191 to Mahaley, issued July 24, 1917 which discloses an automatic gauge glass wiper. Another GAUGE CLEANING DEVICE is disclosed in U.S. Pat. No. 2,206,006 to Hendrey issued June 25, 1940.
Another approach to the same problem is to provide the gauge with a deflector right below its upper gasket so as to carry the steam and condensate away from the surface of the glass itself. An early type of deflector is disclosed in U.S. Pat. No. 1,387,676 issued on Aug. 16, 1921 to P. I. Wright. An improvement in gauge glass deflectors is also disclosed in U.S. Pat. No. 3,862,572 issued on Jan. 28, 1975 to Orlin R. Norris, the inventor of the device disclosed herein.
The devices described in U.S. Pat. Nos. 1,387,676 and 3,862,572 are believed to be satisfactory under general working conditions. However, there still continues to be a need for an effective, inexpensive gauge glass protector which does not possess the disadvantages inherent in the prior art.
While the problems of the prior art discussed above refer to the use of gauge glasses on steam boilers, it will be appreciated by those of ordinary skill in the art that the same sight gauge problems may be equally applicable to oil/ammonia systems such as used in conjunction with refrigeration compressers, holding tanks for cryogenic or freezing liquids, heated or unheated, fired or unfired pressure vessels used at, below or above atomspheric pressure.
SUMMARY OF THE INVENTION
Briefly described the invention comprises an improved gauge glass protector for use on gauge glasses such as found in a steam boiler system. The gauge glass protector, according to the preferred embodiment of the invention, comprises a frustroconical skirt having an up-turned collector rim around the base thereof. The conical skirt includes a hole at the center thereof for accomodating a small rubber gasket having an internal diameter slightly less than the outside diameter of the gauge glass. The protector when used in the deflector mode is preferably located about 1/2 inch below the upper valve body packing nut in an umbrella-like fashion. The steam escaping from the packing nut is deflected down the skirt and collected in the collector rim. At least one small drain hole is located at the junction between the conical skirt and the collector rim for the purpose of carrying the collected liquid away from the glass and letting it fall harmlessly to the floor. A drip wire may be placed in the drip hole in order to conduct the liquid away more efficiently.
By inverting the protector/deflector it is possible to use it as a vapor collector. In this mode the shield in its inverted position is located approximately 1 inch below the upper valve body packing nut. This method is especially effective with very fine escaping aerosol mists which do not contain a great deal of liquid. If the mist is sufficiently fine, the collector will trap the mist and allow it to evaporate before the shield overflows.
According to another embodiment of the present invention the protector skirt may be made from a flat piece of semi-soft material. The flat material is equipped with a tab and slot arrangement so that when the tab engages the slot the skirt assumes a three dimensional conical shape. The advantage of this particular embodiment is that it enables the deflector to be attached to the gauge glass without the necessity of removing the glass from the boiler.
In yet another embodiment the gauge glass protector comprises a helical coil of plastic which by the constriction of its coil elements adheres to the gauge glass near the location of the upper packing nut. The bottom end of the coil includes a straight discharge trough for removing condensate collected by the coil away from the vicinity of the gauge glass. These and other embodiments of the invention will be more fully understood with reference to the drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a conventional sight gauge in position on the side of a vessel.
FIG. 2A is a top plan view of the gauge glass protector according to the preferred embodiment of the present invention.
FIG. 2B is a cross-sectional view of the gauge glass protector illustrated in FIG. 2A, as seen from perspective 2B--2B.
FIG. 3 is an elevational view of the gauge glass protector in position on a sight gauge in its deflector mode and including a drip wire connected thereto.
FIG. 4 is an elevational view illustrating the use of the gauge glass protector in its collector mode.
FIG. 5 illustrates an embodiment in which the gauge glass protector comprises a coiled spring having a straight run-off trough at the bottom thereof.
FIG. 6 illustrates the gauge glass protector of FIG. 5 as shown in position on a sight gauge.
FIG. 7 is a top plan view of an embodiment in which the gauge glass protector skirt is formed from a flat piece of semi-circular material.
DETAILED DESCRIPTION OF THE INVENTION
During the course of this description like numbers will be used to indicate like elements according to the different views of the invention.
Details of a conventional sight gauge 10 can be understood with reference to FIG. 1. For the purposes of this description the terms "sight gauge" and "gauge glass" can be used interchangeably. The gauge glass 10 is typically tubular and transparent and connected via appropriate fittings to a gas/liquid system 12. Gauge glasses are frequently found on steam boilers but may also be employed in a variety of other contexts too numerous to mention individually. The gauge glass protectors described herein are believed to be usable on almost any type of conventional gauge glass.
The gauge glass 10 is connected to the vapor phase of the vessel 12 by means of upper valve 14. In a similar manner, the lower end of the gauge glass 10 is connected through lower valve 16 to the liquid phase of the vessel 12. There are many ways in which the glass 10 may be sealed with respect to the upper and lower valves 14 and 16. However, it is generally preferred that the glass be held in position by means of a sealing gland or basket 18 and a compression nut 20 both of which elements may be seen in partial cross-section with respect to the upper valve 14.
The glass may be removed and replaced by unscrewing the compression nuts 20, dislodging the gaskets 18 and taking the gauge glass 10 out of its receiving sockets. A new glass 10 may be replaced by putting a new gasket 18 at both ends thereof and then compressing the seals 18 against the seats in their respective valve bodies 14 and 16 by means of compression nuts 20. When both valves 14 and 16 are open it is possible to accurately read the level of liquid 22 in the boiler.
Even with the best of materials, it is difficult to avoid having mist or liquid escape from the sealing gasket 18 located in the valve 14. The escape of a fine aerosol or mist 24 is illustrated in FIG. 1. If the seal is weaker then it is likely that droplets of liquid condensate 26 may also escape. In order to minimize the dangers inherent with escaping liquids it has been found desirable to provide the gauge glass 10 with some form of protector.
A gauge glass protector 30 according to the preferred embodiment of the present invention is illustrated in FIGS. 2A and 2B. The protector 30 is shown in a top plan view in FIG. 2A and includes an annular center grommet 32, a frustro-conical skirt 34 and a collector rim 36. A drain hole 38 is located at the juncture of the skirt 34 and the rim 36. The purpose of the drain hole 38 is to discharge liquid trapped in the trough 48 formed between the skirt 34 and the rim 36. Drain hole 38 should be sufficiently far away from the grommet 32 so that the liquid issuing therefrom does not accidentally fall upon the glass gauge itself.
The grommet 32 has an upper tapered surface 40 and a lower tapered surface 42. Intermediate the two tapered surfaces 40 and 42 is a circumferential groove 44 which is adapted to receive the upper annular edge of skirt 34. The upper tapered surface 40 serves to direct liquid downwardly onto the skirt 34. The lowered tapered surface 42 is advantageous when the protector is used in the collector mode as illustrated in FIG. 4. In addition, it is possible to fashion a plurality of grommets 32 from a long piece of grommet tubing material by cutting the tubular stock on a lathe like machine in such a fashion that the lower tapered surface 42 is at the inner face of the upper tapered surface 40 of the next grommet being produced.
According to the preferred embodiment of the invention the grommet material comprises a temperature and chemical resistant rubber or plastic material having an inside diameter 46 which is just slightly smaller than the outside diameter of the gauge glass 10. The skirt 34 and the rim 36 are preferably a continuous piece of lightweight corrosion resistant material such as aluminum. The drain hole 38 should be at least 3/32 inch in diameter. It is important that the drain hole be sufficiently large so that the surface tension of the liquid collected does not prevent the liquid from being discharged from trough 48.
It is desirable that the inner surface of the deflector contact the surface of the gauge glass 10 in such a manner that no leakage is possible between the upper surface 40 and the lower surface 42. This criterion is subject to the fact that absolute heat resistance is not required, however, it is desirable that the material does not disintegrate rapidly at temperatures up to 400° F under repeated exposures of not in excess of 5 minutes per exposure.
While the invention is not limited thereto, it has been found that synthetic rubbers such as, for example, neoprene, teflon, and other rubber compositions are suitable for this purpose. It has also been found that the skirt 34 and collector rim 36 may be made of other materials such as plastic, glass, clay, asbestos and sheet metal.
For a gauge glass having outside diameter of 3/4 inch it might be appropriate to use a grommet 32 having an inside diameter 46 approximately 1/32 inch smaller, or about 23/32 inch. Under such circumstances, it has been found that the outside diameter of the collector rim 36 should be approximately 2 inches and that the center of the drain hole 38 should be located approximately 1/4 inch inside of the outer collector rim 36. In other words, the trough 48 formed between the skirt 34 and the rim 36 is approximately 3/4 inch from the axial center of the protector 30.
A gauge glass protector 30 used in the deflector mode is illustrated in FIG. 3. In this mode the minimum distance between the gasket 32 and the packing nut 20 is approximately 1/2 inch. The grommet 32 should grab onto the surface of the gauge glass 10 with sufficient force to keep the protector 30 in position but not so strongly as to prevent the protector 30 from being moved up and down the surface if necessary. Adjustment may be necessary in order to install the protector 30 and it may be desirable to move the protector 30 from time to time in order to clean off material desposits.
In operation the protector is located on a gauge glass 10 in the manner illustrated in FIG. 3. Liquid such as droplet 26 illustrated in FIG. 1 will roll down the gauge glass 10 and impinge upon the upper surface 40 of the grommet 32. Due to the taper of the upper surface 40 the liquid will be carried onto the frusto-conical skirt 34 and down into trough 48. As liquid is collected between the skirt 34 and the rim 36 it will eventually find its way to drain hole 38 and be discharged away from the surface of the gauge glass 10. In this manner the surface of the gauge glass 10 below the protector 30 is protected from mist 24 and liquids 26 that may leak from the upper seal 18 or that may otherwise form by condensation and so forth above the protector 30. In order to facilitate the drainage of liquid from trough 48 it may be optionally desirable to suspend a drip directing wire 50 through the drain hole 38 in such a manner as to carry the droplets further away from the surface of the gauge glass 10. The drip directing wire 50 is typically bent so that liquid flowing down the wire passes below and free of the lower valve assembly 16, thus directing the droplets of condensate harmlessly away to any chosen area below.
The protector 30 may also be used in a collector mode as illustrated in FIG. 4. In this manner the protector 30 is inverted such that the minimum distance between the inverted protector 30 and the upper packing nut 20 is approximately 1 inch. The protector 30 is especially effective in the collector mode of FIG. 4 when the escaping liquid is in the form of a fine mist 24 as illustrated in FIG. 1. If the fine mist 24 does not include much liquid then the fine mist will impinge upon the inner surface of the conical skirt 34 and will harmlessly evaporate under the influence of the ambient heat. In the collector mode the protector 30 forms a small reservoir for the escaping 24 and also tends to prevent the mist from impinging upon the lower portions of the gauge glass 10.
A helical gauge glass protector 52 is illustrated in detail in FIG. 5. The helical protector 52 preferably comprises a spiral upper body 54 and a discharge trough 56. The spiral body 54 is wound in such a fashion as to be held in position when located on a glass gauge 10 as illustrated in FIG. 6. As in the case with the protector 30 previously described, the helical protector 52 must be manually movable, but must also stay in place under normal operating conditions when not effected by an outside force. The discharge section 56 of the helical protector 52 is a continuation of the spiral body 54 and includes therein a small trough 58. The end of the discharge section 56 is located well away from the body of the gauge glass 10 so that liquid issuing therefrom does not impinge upon the surface of the gauge glass.
In operation, the helical protector is located on the glass gauge in the manner illustrated in FIG. 6. Droplets of liquid which may issue from the packing gasket 18 will impinge upon the spiral body 54 and follow the spiral down the body under the influence of gravity until they arrive at the discharge section 56. The discharge section 56 is tangent to the gauge glass 10 and the travelling droplets will be picked up by the trough 58 located therein. The droplets then continue down the inclined trough where they are discharged at a safe distance away from the surface of the gauge glass 10. The helical compression protector 52 may be manufactured from a variety of known plastic or rubber covered wires or from suitable semielastic plastics. The plastic or rubber material would be selected from one of a variety of materials which are known to operate at the elevated temperatures and conditions at which the surface of the gauge glass 10 is normally subjected.
A flexible collar protector embodiment 60 is illustrated in its flat condition in FIG. 7. The flexible collar 60 includes a semi-circular section 62, a tab section 64, and a tab receiving slot 66. The flexible collar 60 may be attached to a gauge glass 10 by wrapping the semi-circular section 62 around the gauge glass 10 and then inserting tab 64 into tab receiving slot 66. In this manner the flexible collar 60 assumes a frustro-conical shape similar to that of the skirt 34 of protector 30. When in position the flexible collar 60 would be located approximately 1/2 inch below the top packing nut 20. When the flexible collar 60 is assembled, it provides umbrella type protection of the glass gauge 10 in a manner similar to that provided by the conical protector 30. That is to say the droplets 26 and aerosol mist 24 that collect on the surface of the glass will flow down the frustro-conical section 62 to the edge of the protector 60 and then fall harmlessly free of the lower section of the gauge glass thereby protecting its visibility and integrity. A variety of semi-soft rubber or plastic materials known to those of ordinary skill in the art would be suitable to produce the flexible collar 60.
While the invention has been described with reference to a preferred embodiment thereof, it will be appreciated by those of ordinary skill in the art that various changes may be made to the materials and the structure of the invention without departing from the spirit and scope thereof. | A gauge glass protector includes an annular grommet carried by a frustro-conical skirt and an inverted collector rim at the circumference of the skirt. A drainage hole for condensate is located at the juncture of the collector rim and the conical skirt for draining the collected liquid out of the trough formed between the skirt and the rim. The same device may be used as an aerosol mist collector by inverting it. In another embodiment of the invention the skirt may comprise a semi-circular flexible collar which when assembled has a frustro-conical shape. Another embodiment calls for a spiral wire attached to the sight gauge including a conical run-off trough at the point where the wire is tangential to the gauge. | 6 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to provisional application No. 60/865,707 filed on Nov. 14, 2006 and is incorporated herein by reference.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
[0002] Not Applicable.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0003] In the accompanying drawings which form part of the specification:
[0004] FIG. 1 is an exploded view in front elevation of blades, ferrule and set screw of one embodiment of arrowhead of this invention;
[0005] FIG. 2 is a view in rear elevation of the blades and ferrule of FIG. 1 assembled;
[0006] FIG. 3 is a top plan view of the arrowhead of FIG. 2 ;
[0007] FIG. 4 is a sectional view taken along the line 4 - 4 of FIG. 1
[0008] FIG. 5 is an exploded view in front perspective of blades, ferrule and set screws of a second embodiment;
[0009] FIG. 6 is a view in side elevation of the blades and ferrule of FIG. 4 assembled;
[0010] FIG. 7 is a top plan view of the arrowhead of FIG. 5 ;
[0011] FIG. 8 is an exploded view in front elevation of a third embodiment;
[0012] FIG. 9 is a view in rear elevation of the ferrule of FIG. 8 ;
[0013] FIG. 10 is an exploded view in front perspective of a fourth embodiment; and
[0014] FIG. 11 is a view in rear elevation of the ferrule of FIG. 10 .
[0015] Corresponding reference numerals indicate corresponding parts throughout the several figures of the drawings.
DESCRIPTION OF THE PREFERRED EMBODIMENT
[0016] The following detailed description illustrates the invention by way of example and not by way of limitation. The description clearly enables one skilled in the art to make and use the invention, describes several embodiments, adaptations, variations, alternatives, and uses of the invention, including what is presently believed to be the best mode of carrying out the invention.
[0017] In the first embodiment of the present invention, referring to FIG. 1 , a blade slot 2 is formed in a ferrule 1 with an upper open end 3 and lower closed end 4 . A blade slot 5 is also formed in ferrule 1 with an upper open end 6 and lower closed end 7 . The slots 2 and 5 are formed with axes at right angles to one another. As a result of the provision of the blade slots 2 and 5 , the ferrule 1 has a body 100 and four segments 101 , 102 , 103 , and 104 . Segment 101 has hole 8 , which may or may not be internally threaded, depending upon the kind of set screw 15 used, whose axis is transverse to the longitudinal axis of the ferrule 1 , at a point between upper open end 3 and lower closed end 4 . Segment 102 has a transverse, internally threaded hole 108 , aligned with the hole 8 . A blade slot, 9 is provided in a blade 10 . Transverse hole 11 forms a central opening through blade 10 . A blade slot 12 forms an opening in blade 13 . Transverse hole 14 forms a central opening through blade 13 . As can be seen, the slot 12 extends through the upper edge of the blade 13 , while the slot 9 extends through the lower edge of the blade 10 , the two blade slots being aligned when installed. Blades 10 and 13 are inserted into slots 2 and 5 , and interengage with one another. Set screw 15 is shown as being threaded at its outer end 16 with a smooth shank 17 and a conical slotted head 18 . The head 18 seats in a countersunk seat 19 at the entrance of hole 8 . Alternatively, the hole 8 can be made sufficiently large to permit the passage of the threaded part of a fully threaded type set screw, or threaded. In any case, the set screw is pushed or screwed through transverse ferrule hole 8 , passing through blade hole 11 in blade 10 , and blade hole 14 in blade 13 , and is screwed into internally threaded hole 108 , securing blades 10 and 13 in alignment in the ferrule.
[0018] Referring to FIG. 2 , the parts of FIG. 1 are assembled showing the complete arrowhead.
[0019] Referring to FIG. 3 , the orientation of the ferrule, blades and screw attachment is shown.
[0020] Referring to FIG. 4 , the passage of the set screw 15 through the blades 10 and 13 is illustrated.
[0021] Referring to FIG. 5 , for a second embodiment, a ferrule 20 includes a slot 21 with an upper open end 22 and lower closed end 23 . Ferrule 20 also includes a slot 24 with an upper open end 25 and lower closed end 26 , oriented at right angles to the slot 21 . As with the embodiment shown in FIGS. 1-3 , the slots 21 and 24 define four segments, opposite ones of which, in this embodiment, have aligned holes in them. One pair of segments has aligned holes 27 and 31 whose axes are transverse to the longitudinal axis of the ferrule 20 . Hole 31 is threaded. The hole 27 can be threaded or unthreaded, as has been described above. The other pair of segments has holes 27 ′ and 31 ′, whose axes are also perpendicular to the longitudinal axis of the ferrule 20 , but positioned closer to the tip of the segments than the holes 27 and 31 , sufficiently far as to accommodate a second set screw. In this embodiment, the exterior surfaces of the segments of the ferrule 20 are concave. Slot 81 forms an opening in blade 29 . Transverse hole 28 forms an opening through blade 29 . Transverse hole 30 forms another opening through blade 29 . Slot 82 forms an opening in blade 34 . Transverse hole 33 forms an opening through blade 34 . Transverse hole 35 forms another opening through blade 34 . Blades 29 and 34 are inserted into slots 21 and 24 , and interengage. Set screw 36 is applied to transverse ferrule hole 27 , passing through blade hole 28 in blade 29 , and blade hole 33 in blade 34 , securing blades 29 and 34 in alignment. Set screw 37 is applied to transverse ferrule hole 31 , passing through blade hole 30 in blade 29 , and blade hole 35 in blade 34 , further securing blades 29 and 34 in alignment. As is the case in the embodiment shown in FIGS. 1-3 , the screws holding the blades can either be fully threaded or threaded only at their ends, in the latter case, with a smooth shank passing through the initial hole, and a head, preferably countersunk, to limit the travel of the screw, and permit its tightening.
[0022] Referring to FIG. 6 , the parts of FIG. 4 are shown assembled to form the complete arrowhead.
[0023] Referring to FIG. 7 , the orientation of the ferrule, blades and screw attachments is shown.
[0024] Referring to FIG. 8 , ferrule 38 includes slot 39 with an upper open end 40 and lower closed end 41 . Ferrule 38 also includes a slot in the form of an aperture 42 with an upper closed end 43 and closed lower end 44 , oriented at right angles to the slot 39 . Ferrule 38 has a hole 45 whose axis is transverse to the longitudinal axis of the ferrule 38 , and an aligned, internally threaded hole 45 ′ on the other side of the slot 39 . Transverse slot 95 forms an opening in blade 47 . Transverse hole 46 forms an opening through blade 47 . Transverse hole 48 forms an opening through blade 49 . Blade 47 is inserted in slot 39 and blade 49 is then inserted in slot 42 , interengaging blade 47 . Set screw 50 is applied to transverse ferrule hole 45 , passing through blade hole 46 in blade 47 and blade hole 48 in blade 49 , and screwing into internally threaded hole 45 ′, securing blades 47 and 49 in alignment.
[0025] Referring to FIG. 9 , the ferrule of FIG. 8 is shown with the internally threaded hole 45 ′ is shown.
[0026] Referring t FIG. 10 , a ferrule 51 includes slot 52 with an upper open end 53 and lower closed end 54 . Ferrule 51 also includes a slot in the form of an aperture 55 with an upper closed end 56 and closed lower end 57 . Ferrule 51 has a hole 58 whose axis is transverse to the longitudinal axis of the ferrule 51 , and an internally threaded hole 58 ′ on the opposite side of the slot 52 . Slot 61 in blade 62 has a closed upper end 68 and an open lower end 69 and passes through the central axis of the blade 62 . Transverse hole 60 forms an opening through blade 62 . Slot 59 in blade 64 has an open upper end 70 and a closed lower end 71 . Transverse hole 63 forms a second opening through blade 64 . Blade 64 is inserted in slot 55 , and blade 62 is then inserted in slot 52 interengaging blade 64 . Set screw 66 is pushed or screwed through transverse hole 58 , passing through blade hole 60 in blade 62 and blade hole 63 in blade 64 , and screwed into hole 58 ′, securing blades 62 and 64 in alignment.
[0027] FIG. 11 shows internally threaded hole 58 ′.
[0028] The set screws 15 , 36 , 37 , and 50 are preferably made with a head fitting in a countersink in the hole to which it is introduced, that hole being unthreaded and slightly larger than an unthreaded part of the shank of the screw, the screw being threaded at its outer section that engages threads in the other hole as has been illustrated and described. In this way the screw tends to clamp the blade when it is tightened, and at the same time, it is easier to insert. However, the holes can both be threaded, as can the entire shank of the screw.
[0029] Numerous variations in the construction of the broadhead of this invention will occur to those skilled in the art in the light of the foregoing disclosure. The external shapes or dimensions of the blades and the angles of the sharp edges can be varied. The sets of slots may be offset from one another longitudinally. The blades may be offset at an angle relative to the ferrule. The body of the ferrule and the tip can be made polygonal, rather than smoothly cylindrical, with flat, concave, or convex sides. The terminal portion of the ferrule may also include numerous fittings besides the threaded shank. The blades may have top ends that are blunt, recessed or pointed. The blades edges may be straight or irregular, such as serrated. The ferrule slots need not be symmetrical in longitudinal orientation nor are the ferrule slots necessarily the same longitudinal length. The slots may be different widths in respect to one another. The blades may be the same or different length, width or height with respect to one another. The ferrule slots may be formed at an angle other than 90 degrees with respect to each other, for instance 120 degrees. One or both blade tips may extend forward from the ferrule, be flush with the ferrule, or be contained within the ferrule. If a heavier arrowhead is desired, the ferrule can be made longer. Mounting means other than screws can be employed, as a key slot or bayonet type member. Although the head of the screws illustrated are slotted, they can be provided with a Phillips head or other such head. If the blades are not to be replaced, the mounting means can be a rivet, although that is not a preferred variation. These are merely illustrative.
[0030] In view of the above, it will be seen that the several objects of the invention are achieved and other advantageous results are obtained. As various changes could be made in the above constructions without departing from the scope of the invention, it is intended that all matter contained in the above description or shown in the accompanying drawings shall be interpreted as illustrative and not in a limiting sense. | A broadhead includes a one piece elongated ferrule, with a plurality of slots through a central longitudinal axis of said ferrule, at least one of which has an open end, and one piece blades mounted in the slots. At least one of the blades includes a blade slot in it and the blades having openings through them. A securing member is inserted transversely through the central longitudinal axis of the ferrule and passes through said openings through the openings of the blades securing them within the ferrule. | 5 |
FIELD OF THE INVENTION
The present invention relates to catheters used to return oxygenated blood from a cardiopulmonary bypass machine to a patient during cardiac surgery. More specifically, the present invention relates to a perfusion catheter, and methods of use, that enable the catheter to be intraoperatively placed in the aorta using a sutureless arteriotomy seal.
BACKGROUND OF THE INVENTION
Each year hundreds of thousands of people are afflicted with vascular diseases, such as arteriosclerosis, that result in cardiac ischemia. For more than thirty years, such disease, especially of the coronary arteries, has been treated using open surgical procedures, such as coronary artery bypass grafting. During such bypass grafting procedures, a sternotomy is performed to gain access to the pericardial sac, the patient is put on cardiopulmonary bypass, and the heart is stopped using a cardioplegia solution.
More recently, techniques are being developed, for example, by Heartport, Inc., Redwood City, Calif., that permit cardiac surgery using an endoscopic approach, in which small access openings are created between the ribs. The bypass graft or heart valve repair procedure is performed guided by an image displayed on a video monitor. In the “keyhole” techniques developed by Heartport, the patient's heart is stopped and the patient is placed on cardiopulmonary bypass. Still other techniques being developed, for example, by CardioThoracic Systems, Inc., of Cupertino, Calif., enable such bypass graft procedures to be performed on a beating heart.
In those techniques that involve stopping the heart to perform surgery, blood flow to the heart is occluded, for example, by placing occlusion balloons in the ascending aorta and/or the vena cava. Venous blood is then withdrawn from the patient, for example, from the vena cava, and oxygenated using an extracorporeal oxygenation circuit. The oxygenated blood is perfused into the patient in the vicinity of the aortic arch to provide oxygenated blood to the brain, internal organs and extremities.
U.S. Pat. No. 5,312,344 to Grinfeld et al. describes a multi-lumen perfusion catheter for perfusing oxygenated blood into a patient on cardiopulmonary bypass. The catheter has a distal balloon for occluding the ascending aorta, a first lumen for delivering cardioplegia solution through a first opening distal to the balloon, and a second lumen for perfusing oxygenated blood through a second opening proximal to the balloon. The catheter may be positioned in the ascending aorta either intraoperatively through an opening in the aorta, or in a retrograde manner via a femoral artery and the abdominal aorta.
One drawback associated with recently developed keyhole methods of cardiac surgery is that the surgeon often has only limited room in which to maneuver. This, in turn, may render previously known apparatus too cumbersome to be effectively used in conjunction with such techniques. Thus, for example, while the intraoperative version of the catheter described in the foregoing patent to Grinfeld et al. may be used instead of a cross-clamp where a sternotomy has been performed, the device may be less useful when keyhole surgical techniques are employed.
Specifically, intraoperative placement of the foregoing catheter involves placing a purse-string suture surrounding the arteriotomy, to prevent excessive blood loss. Because there may be insufficient room in which to form a purse string suture in a keyhole-type procedure, the surgeon may be unable to provide a tight seal around the entry point of the catheter.
It therefore would be desirable to provide apparatus and methods for delivering oxygenated blood to a patient from a cardiopulmonary bypass machine that overcome the drawbacks of previously known perfusion catheters.
It further would be desirable to provide apparatus and methods that enable a perfusion catheter to be positioned in the aorta via a sutureless arteriotomy.
A number of devices and methods have been developed to provide sutureless anastomoses. U.S. Pat. Nos. 4,366,819 and 4,368,736, both to Kaster, describe assemblies that provide sutureless anastomosis of a bypass graft by capturing the graft material between an interior flange and an exterior ring. U.S. Pat. No. 4,352,358 to Angelchik describes an anastomosis device formed from a tubular elastic membrane that is expanded on either side of the entry wound to provide a sutureless seal. None of these previously known devices appear suitable, without extensive modification, for providing a temporary sutureless arteriotomy for a perfusion catheter.
U.S. Pat. No. 5,167,628 to Boyles describes a catheter for isolating the coronary ostium between two toroidal-shaped balloons. The catheter includes a lumen enabling blood to pass from the left ventricle to the ascending aorta, while the balloons define a chamber into which treatment material may be provided to the coronary arteries. The patent describes that the balloons are spaced apart so that the lower balloon is disposed beneath the aortic valve in the left ventricle and the upper balloon is positioned distal of the coronary arteries.
In view of the foregoing, it would be desirable to provide apparatus and methods for delivering oxygenated blood to a patient from a cardiopulmonary bypass machine using sealing members that provide a sutureless arteriotomy, with little or no blood leakage.
It further would be desirable to provide apparatus and methods for occluding the aorta and for providing cardioplegia solution to the aortic root using a perfusion catheter inserted via a sutureless arteriotomy.
SUMMARY OF THE INVENTION
In view of the foregoing, it is an object of this invention to provide apparatus and methods for delivering oxygenated blood to a patient from a cardiopulmonary bypass machine, and that overcome the drawbacks of previously known perfusion catheters.
It is a further object of the present invention to provide apparatus and methods that enable a perfusion catheter to be positioned in the ascending aorta via a sutureless arteriotomy.
It is another object of this invention to provide apparatus and methods for delivering oxygenated blood to a patient from a cardiopulmonary bypass machine using sealing members that provide a sutureless arteriotomy, with little or no blood leakage.
It is a further object of the present invention to provide apparatus and methods for occluding the aorta and for providing cardioplegia solution to the aortic root using a perfusion catheter inserted via a sutureless arteriotomy.
These and other objects of the invention are accomplished by providing a perfusion catheter having a distal end carrying first and second sealing members. When the perfusion catheter is inserted through an arteriotomy site, the first and second sealing members are disposed to engage opposite surfaces of a thickness of a vessel wall. When disposed across a vessel wall, the first and second sealing members capture the intervening tissue and apply pressure against the opposite surfaces of the thickness of the vessel wall to seal blood perfused into the aorta from leaking through the arteriotomy site.
In one embodiment, the perfusion catheter includes a multi-lumen catheter having first and second toroidal balloons defining first and second sealing members, a third balloon for occluding the aorta, a lumen for providing oxygenated blood to the aorta, and a lumen for injecting cardioplegia solution into the aortic root, proximal of the occlusion balloon. Alternatively, the third balloon and cardioplegia injection lumen may be carried on a separate catheter that is inserted through a lumen of the perfusion catheter. The distal region of the catheter also may include a member that biases the perfusion catheter into a preferred delivery shape when deployed, e.g., with the axis of a blood flow outlet port coinciding with the axis of the aorta. A stylet for forming the arteriotomy puncture and inserting the perfusion catheter also is provided.
In an alternative embodiment, the perfusion catheter comprises a multi-lumen catheter having an inner shaft including a toroidal balloon defining a first sealing member, an occlusion balloon for occluding the aorta, a lumen for providing oxygenated blood to the aorta, and a lumen for injecting cardioplegia solution into the aortic root, proximal of the occlusion balloon. An outer shaft is disposed for movement in the proximal and distal directions on the inner shaft and includes an elastomeric flange or toroidal balloon defining a second sealing member. Once the first balloon is positioned and inflated, the outer shaft is advanced in the distal direction to engage the tissue disposed therebetween and seal the arteriotomy.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features of the invention, its nature and various advantages will be more apparent from the accompanying drawings and the following detailed description of the preferred embodiments, in which:
FIG. 1 is a side view of an illustrative embodiment of a perfusion catheter system constructed in accordance with the present invention;
FIG. 2 is a perspective view of the distal end of the perfusion catheter system of FIG. 1 disposed in a patient's aortic arch;
FIG. 3 is a side-sectional view of the distal end of the perfusion catheter system of FIG. 2;
FIGS. 4A to 4 C illustrate a method of placing the distal end of the perfusion catheter of FIG. 1 in an aortic arch;
FIG. 5 is a side view of an alternative embodiment of a perfusion catheter system constructed in accordance with the present invention;
FIG. 6 is a perspective view of the distal end of the perfusion catheter system of FIG. 5 disposed in a patient's aortic arch;
FIG. 7 is a side-sectional view of the distal end of the perfusion catheter of FIG. 6;
FIG. 8 is a cross-sectional view of the perfusion catheter of FIG. 5, taken along view line 8 — 8 of FIG. 7;
FIG. 9 is a side view of an alternative embodiment of a perfusion catheter system constructed in accordance with the present invention;
FIGS. 10A and 10B are perspective views of the distal end of the perfusion catheter system of FIG. 9 showing steps of deploying the catheter in a patient's aortic arch; and
FIG. 11 is a side-sectional view of the distal end of the perfusion catheter of FIG. 9 .
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a perfusion catheter that may be positioned in a patient's aorta without suturing the arteriotomy site, and with little or no leakage. Specifically, perfusion catheters constructed in accordance with the principles of the present invention include first and second sealing members disposed on the catheter shaft in closely spaced relation that sealingly capture the edge of the arteriotomy site. In addition, the perfusion catheters of the present invention may include an inflatable occlusive member for occluding retrograde flow of blood into the heart, a lumen for delivering cardioplegia solution to the aortic root, and an element that causes the distal end of the perfusion catheter to conform to the vessel.
Referring to FIGS. 1 to 3 , an illustrative perfusion catheter system constructed in accordance with the principles of the present invention is described. Catheter system 10 comprises perfusion catheter 20 , balloon catheter 40 and stylet 50 .
Perfusion catheter 20 comprises flexible tube 21 having proximal end 22 and distal end 23 . Proximal end 22 includes fitting 24 for coupling blood flow inlet port 25 to an outlet of a cardiopulmonary bypass machine (not shown). Distal end 23 includes tube 26 , closely-spaced together sealing members 27 and 28 , and curved region 29 having blood flow outlet port 30 . Lumen 31 (see FIG. 3) extends from blood flow inlet port 25 to blood flow outlet port 30 . Tube 26 is affixed to the exterior surface of perfusion catheter 20 and forms a guide lumen for balloon catheter 40 , as described hereinbelow. Sealing members 27 and 28 comprise toroidal balloons, and are coupled to inflation ports 32 and 33 , respectively, via separate lumens 34 disposed within lumen 31 . Inflation ports 32 and 33 may be coupled to syringes (not shown) filled with an inflation medium, such as saline, to selectively inflate the balloons.
Perfusion catheter 20 preferably comprises a material typically used in catheter construction, such as polyethylene, polyvinylchloride, or polyurethane. Curved region 29 preferably includes pre-formed metal alloy spring 35 embedded in its thickness (see FIG. 3 ). Spring 35 flexes from a substantially straight shape, when perfusion catheter 20 is disposed over stylet 50 , to a curved shape that conforms to the arch of the aorta, as shown in FIGS. 2 and 3. Sealing members 27 and 28 may comprise a compliant, semi-compliant, or non-compliant material, and more preferably, a non-compliant or semi-compliant material. Tube 26 may include a thin seal of a plastic material, e.g., polyethylene, which is punctured when balloon catheter 40 is inserted through the tube.
Balloon catheter 40 has proximal end 41 and distal end 42 . Proximal end 41 includes cardioplegia inlet port 43 and inflation port 44 . Distal end 42 includes outlet port 45 coupled via lumen 46 (see FIG. 3) to cardioplegia inlet port 43 , and balloon 47 coupled via a lumen to inflation port 44 . Balloon catheter 40 has a diameter selected so that distal end 42 passes through tube 26 of perfusion catheter 20 when balloon 47 is deflated, and may include one or more additional lumens, for example, for venting the aortic root. Balloon catheter 40 preferably comprises a material typically used in catheter construction, such as polyethylene, polyvinylchloride, or polyurethane, while balloons 47 may comprise a compliant, semi-compliant, or non-compliant material, and more preferably, a compliant material.
Stylet 50 comprises elongated shaft 51 having knob 52 at proximal end 53 and sharpened non-coring tip 54 at distal end 55 . Stylet 50 is sized to slidingly fit within lumen 31 of perfusion catheter 20 , and may comprise a catheter type material, such as described hereinabove. Stylet 50 may include grooves in its outer surface to accommodate the presence of lumens 34 in lumen 31 of perfusion catheter 20 . In addition, tip 55 may include a sharpened metal alloy tip embedded in distal end 55 to enhance the cutting ability of the stylet.
Referring now to FIGS. 2 and 3, when perfusion catheter 20 is positioned within a vessel, preferably aorta A, for example, during keyhole cardiac surgery, curved region 29 conforms to the curve of the aorta. Sealing member 28 is disposed within aorta A and contacts the interior surface of tissue T of the vessel wall. Sealing member 27 is disposed outside aorta A and contacts the exterior surface of tissue T of the vessel wall. When sealing members 27 and 28 are inflated, e.g., when the surgeon injects a suitable inflation medium in sealing members 27 and 28 via inflation ports 32 and 33 , the balloons expand to bear against opposite surfaces of the thickness of tissue T. Sealing members 27 and 28 thereby occlude and seal the arteriotomy site against leakage, without the need to place a purse string suture around the catheter.
Balloon catheter 40 is advanced through tube 26 along a guide wire, and balloon 47 is inflated using a suitable inflation medium to occlude the aorta. Cardioplegia solution then may be injected through cardioplegia inlet port 43 , lumen 46 and cardioplegia outlet port 45 into the aortic root to stop the heart and perfuse the coronary arteries.
Referring now to FIGS. 4A to 4 C, a method of intraoperatively using perfusion catheter system 10 of the present invention to perfuse a patient undergoing cardiac surgery with oxygenated blood is described. As shown in FIG. 4A, a portion of aorta A is first partially clamped using previously known forceps-type cross-clamp 55 to isolate a region in which the arteriotomy is to be performed.
Perfusion catheter 20 is placed over stylet 50 so that tip 54 extends out of blood flow outlet port 30 . Sealing members 27 and 28 are folded, and preferably pre-folded, flat against the exterior of perfusion catheter 20 so as to minimize the insertion profile of the catheter. Perfusion catheter 20 and stylet 50 are disposed adjacent to the isolated region of the aorta, and the stylet is advanced to create puncture P in the vessel wall, as shown in FIG. 4 B. Perfusion catheter 20 is then advanced over distal end 55 of the stylet with the stylet held stationary.
As the perfusion catheter is inserted into the aorta through puncture P, spring 35 causes curved region 29 to revert to its curved shape, thus allowing the perfusion catheter to be placed in the aorta without contacting the opposing wall of the vessel, as shown in FIG. 4 C. Sealing members 27 and 28 then are inflated (only sealing member 28 is shown inflated in FIG. 4 C), until the balloons contact the opposite surfaces of the intervening thickness of the vessel wall (see FIG. 3 ).
Once sealing members 27 and 28 have been inflated to seal puncture P, balloon catheter 47 is inserted through tube 26 and directed in a retrograde fashion, for example, using a guide wire inserted through lumen 46 and cardioplegia outlet port 45 of balloon catheter 40 . Balloon 47 then is inflated to occlude the aorta upstream of blood flow outlet port 30 of perfusion catheter 20 . Stylet 50 is removed from lumen 31 , and blood flow inlet port 25 is coupled to an outlet of a cardiopulmonary bypass machine to perfuse aorta A, while cardioplegia solution is injected through lumen 46 of balloon catheter 40 .
Referring now to FIGS. 5 to 8 , an alternative embodiment of a perfusion catheter system constructed in accordance with the principles of the present invention is described. Catheter system 60 comprises perfusion catheter 65 and stylet 85 .
Perfusion catheter 65 comprises flexible tube 66 having proximal end 67 and distal end 68 . Proximal end 67 includes fitting 69 for coupling blood flow inlet port 70 of the perfusion catheter to an outlet of a cardiopulmonary bypass machine (not shown). Distal end 68 includes closely-spaced together sealing members 71 and 72 , curved region 73 having cardioplegia outlet ports 74 , occlusion balloon 75 and blood flow outlet port 76 . Lumen 77 (see FIG. 7) extends from blood flow inlet port 70 to blood flow outlet port 76 .
Sealing members 71 and 72 , preferably balloons, and occlusion balloon 75 , are coupled to inflation ports 78 , 79 and 80 , respectively, via separate lumens 81 disposed within lumen 77 . Inflation ports 78 , 79 and 80 may be coupled to syringes (not shown) filled with an inflation medium, such as saline, to selectively inflate the balloons. Cardioplegia outlet ports 74 are coupled to cardioplegia inlet port 82 via lumen 83 disposed within lumen 77 .
Perfusion catheter 65 preferably comprises a material, as described hereinabove with respect to the embodiment of FIGS. 1-4, and includes pre-formed metal alloy spring 84 embedded in its thickness. Spring 84 flexes from a substantially straight shape, when perfusion catheter 65 is disposed over stylet 85 , to a curved shape that conforms to the arch of the aorta, as shown in FIGS. 6 and 7. Sealing members 71 and 72 and occlusion balloon 75 may comprise a compliant, semi-compliant, or non-compliant material, and more preferably, sealing members 71 and 72 comprise a non-compliant or semi-compliant material, while occlusion balloon 75 more preferably comprises a compliant material.
Stylet 85 is similar in construction to stylet 50 described hereinabove, and comprises elongated shaft 86 having knob 87 at proximal end 88 and sharpened non-coring tip 89 at distal end 90 . Stylet 85 is sized to slidingly fit within lumen 77 of perfusion catheter 65 , and may comprise a catheter type material, such as described hereinabove. Stylet 85 may include grooves to accommodate the presence of lumens 81 and 83 , and tip 89 optionally may include a sharpened metal alloy tip embedded in distal end 90 to enhance the cutting ability of the stylet.
Referring to FIGS. 6 and 7, when perfusion catheter 65 is positioned within a vessel, preferably aorta A, curved region 73 conforms to the curve of the aorta. Sealing member 72 is disposed within aorta A and contacts the interior surface of tissue T, while sealing member 71 is disposed outside aorta A and contacts the exterior surface of tissue T. When sealing members 71 and 72 are inflated, the balloons expand to bear against the opposite surfaces of the thickness of tissue T, thus providing a sutureless arteriotomy seal for perfusion catheter 65 .
Operation of catheter system 60 is similar to that described with respect to FIGS. 4A to 4 C. The aorta is first partially clamped to isolate a region in which the arteriotomy is to be performed, and perfusion catheter 65 is placed over stylet 85 so that tip 89 extends out of blood flow outlet port 76 . Sealing members 71 and 72 occlusion balloon 75 are pre-folded flat against the exterior of perfusion catheter 65 so as to minimize the insertion profile of the catheter. The perfusion catheter and stylet are disposed adjacent to the isolated region of the aorta, and the stylet is advanced to create a puncture in the vessel wall.
The perfusion catheter is then advanced over distal end 90 of the stylet with the stylet held stationary, so that spring 84 causes curved region 73 to revert to its curved shape as the perfusion catheter is inserted into the aorta through the puncture. Sealing members 71 and 72 are inflated until the balloons contact and bear against the intervening thickness of the vessel wall. Occlusion balloon 75 also is inflated using a suitable inflation medium, injected via inflation port 80 , to occlude the aorta upstream of blood flow outlet port 76 .
Stylet 85 is removed from lumen 77 , and blood flow inlet port 70 is coupled to an outlet of a cardiopulmonary bypass machine to perfuse aorta A. Cardioplegia solution also may be injected through cardioplegia inlet port 82 , lumen 83 and cardioplegia outlet ports 74 into the aortic root to stop the heart and perfuse the coronary arteries.
Referring now to FIGS. 9 to 11 , a further alternative embodiment of a perfusion catheter system constructed in accordance with the principles of the present invention is described. Catheter system 90 comprises perfusion catheter 95 and stylet 125 . Stylet 125 is constructed as described hereinabove.
Perfusion catheter 95 comprises inner shaft 96 having proximal end 97 and distal end 98 . Proximal end 97 includes fitting 99 for coupling blood flow inlet port 100 of the perfusion catheter to an outlet of a cardiopulmonary bypass machine (not shown). Distal end 98 includes sealing member 101 , curved region 102 having cardioplegia outlet ports 103 , occlusion balloon 104 and blood flow outlet port 105 . Lumen 106 (see FIG. 11) extends from blood flow inlet port 100 to blood flow outlet port 105 . Outer shaft 107 is disposed for movement in the proximal and distal directions on inner shaft 96 and includes sealing member 108 on distal end 109 and locking ring 110 on proximal end 111 . Locking ring 110 may be configured to engage optional threads 112 disposed on the exterior surface of inner shaft 96 , and serves to lock outer shaft 107 in at a desired position relative to inner shaft 102 .
Sealing member 101 , preferably a toroidal balloon, and occlusion balloon 104 , are coupled to inflation ports 113 and 114 , respectively, via separate lumens 115 disposed within lumen 106 (see FIG. 11 ). Inflation ports 113 and 114 may be coupled to syringes (not shown) filled with an inflation medium, such as saline, to selectively inflate the balloons. Cardioplegia outlet ports 103 are coupled to cardioplegia inlet port 116 via lumen 117 disposed within lumen 106 . Sealing member 108 may comprise a flange formed from an elastomeric or closed-cell foam material. Alternatively, sealing member 108 may comprise an inflatable toroidal balloon, in which case outer shaft 107 will include an inflation port and inflation lumen.
Perfusion catheter 95 preferably comprises a material, as described hereinabove, and includes a preformed metal alloy spring embedded in its thickness that flexes from a substantially straight shape, when perfusion catheter 95 is disposed over stylet 125 , to a curved shape that conforms to the arch of the aorta, as shown in FIGS. 10 . Sealing member 101 and occlusion balloon 104 may comprise a compliant, semi-compliant, or non-compliant material, and more preferably, sealing member 101 comprises a non-compliant or semi-compliant material, while occlusion balloon 104 more preferably comprises a compliant material. Sealing member 108 may comprise a non-compliant or semi-compliant balloon, or elastomeric or foam material.
Referring now to FIGS. 10A and 10B, when perfusion catheter 95 is positioned within a vessel, preferably aorta A, curved region 102 conforms to the curve of the aorta. Sealing member 101 is disposed within aorta A and is inflated to contact the interior surface of tissue T. Outer shaft is then translated in the distal direction so that sealing member 108 is disposed against the exterior surface of tissue T, and locking ring 110 is actuated to lock the outer shaft in a fixed position relative to inner shaft 96 . If sealing member 108 is a balloon, it is inflated to bear against the opposite surfaces of the thickness of tissue T. If sealing member 108 is non-expandable, translation of sealing member 108 toward sealing member 101 causes the sealing members to bear against the opposite surfaces of the thickness of tissue T, thus providing a sutureless arteriotomy seal for perfusion catheter 95 .
Operation of catheter system 90 is similar to that described with respect to FIGS. 4A to 4 C. The aorta is first partially clamped to isolate a region in which the arteriotomy is to be performed, and perfusion catheter 95 is placed over stylet 125 so that the tip of the stylus extends out of blood flow outlet port 105 . Sealing member 101 and occlusion balloon 104 are folded against the exterior of perfusion catheter 95 so as to minimize the insertion profile of the catheter. The perfusion catheter and stylet are disposed adjacent to the isolated region of the aorta, and the stylet is advanced to create a puncture in the vessel wall.
The perfusion catheter is then advanced over the distal end of the stylet with the stylet held stationary, so that curved region 102 reverts to its curved shape as the perfusion catheter is inserted into the aorta through the puncture. Sealing member 101 is inflated, and then sealing member 108 is advanced distally to contact and bear against the intervening thickness of the vessel wall. Alternatively, outer shaft 107 may be positioned relative to inner shaft 96 prior to inflation of the sealing member or members. Occlusion balloon 104 also is inflated using a suitable inflation medium, injected via inflation port 114 , to occlude the aorta upstream of blood flow outlet port 105 .
Stylet 125 is removed from lumen 106 , and blood flow inlet port 100 is coupled to an outlet of a cardiopulmonary bypass machine to perfuse aorta A. Cardioplegia solution also may be injected through cardioplegia inlet port 116 , lumen 117 and cardioplegia outlet ports 103 into the aortic root to stop the heart and perfuse the coronary arteries.
As a further alternative embodiment, perfusion catheter system 95 may omit lumen 117 , cardioplegia outlet ports 103 and occlusion balloon 104 . In this case, perfusion catheter 95 may include a tube (similar to tube 26 of the embodiment of FIG. 1) affixed to inner shaft 96 , within sealing member 101 , and over which sealing member 108 is slidably disposed. In this embodiment, a separate balloon catheter, such as balloon catheter 40 of FIG. 1, may be inserted through the tube to provide the occlusion and cardioplegia injection functions described hereinabove with respect to the embodiment of FIG. 1 .
While preferred illustrative embodiments of the invention are described above, it will be apparent to one skilled in the art that various changes and modifications may be made therein without departing from the invention, and it is intended in the appended claims to cover all such changes and modifications which fall within the true spirit and scope of the invention. | Apparatus and methods are provided for delivering oxygenated blood to a patient undergoing cardiac surgery using a perfusion catheter having a distal end carrying first and second sealing members. When the perfusion catheter is inserted through an arteriotomy site, the first and second sealing members are disposed to engage opposite surfaces of a thickness of a vessel to apply pressure against the opposite surfaces of the thickness to seal blood perfused into the vessel from leaking through the arteriotomy site. Apparatus for placing the perfusion catheter, and methods of using the apparatus also are provided. | 0 |
TECHNICAL FIELD
[0001] The present invention relates to a door guide frame for guiding the sliding movement of a roller device which supports a sliding window and provides a sliding opening/closing operation and, more particularly, to a sliding window installation structure which is capable of: stably supporting and moving a sliding window or a horizontal sliding window (hereinafter, generally referred to as a “sliding window”) on a bottom surface and a top surface on which the sliding window is installed; reducing an installation space by minimizing the size of a door guide frame and a roller device for supporting a heavy sliding window, thereby obtaining a wider open view when applied to a window; and employing a structure which prevents a door guide rail from protruding upward from the bottom surface of a window frame so as to prevent occurrence of a passage obstacle which may be caused when the door guide rail protrudes on a moving passage while the window is opened, as well as to provide a good aesthetic appearance, thereby providing excellent applicability to various fields.
BACKGROUND ART
[0002] In general, according to conventional configurations of a door sash (which is configured to install a window glass panel therein and hereinafter, will be described with reference to a door provided with a glass panel, i.e. a window) and a door guide frame (which is installed on a wall surface, a bottom surface, a ceiling surface, or the like so that the door sash is installed inside the door guide frame to be slidingly guided and thus opened/closed) which constitute a sliding window system which is most commonly used as a window system in most of buildings in consideration of cost reduction including efficiency of an opening/closing space and easy installation, as illustrated in FIGS. 1 and 2 , a roller guide rail 1 a is provided on the door guide frame 1 (also referred to as a “window frame”), and a roller 4 r is installed on a lower part of the door sashes 4 a and 4 b in which a glass panel 4 g is put, thereby providing a structure in which a sliding window 4 is slid along the roller guide rail 1 a.
[0003] In such a structure, the roller 4 r below a lower door sash 4 a is slid while supporting the weight of the sliding window 4 on the roller guide rail 1 a , and a sliding guide recess formed on an upper door sash 4 b is guided along an upper guide rail 1 b installed on the upper surface of the window frame 1 while supporting the upper end of the sliding window 4 so that the sliding window 4 may be smoothly moved to be opened/closed while being prevented from falling down.
[0004] In the above described sliding window system having the conventional structure of the prior art as illustrated in FIGS. 1 and 2 , since the door sashes 4 a and 4 b supporting the glass panel 4 g are configured to support the four sides of the glass panel 4 g , it is impossible to secure a wide open view due to the interference of the door sashes 4 a and 4 b . Therefore, as an alternative structure for this, recently, the phenomenon of reducing the open view through the sliding window 4 due to the door sashes 4 a and 4 b illustrated in FIGS. 1 and 2 described above is minimized by adopting the following structure: a sliding window 4 is configured by placing the glass panel 4 g directly on a roller 4 r member without a separate door sash which supports the glass panel 4 g at the four sides of top and bottom, left and right of the glass panel 4 g , as illustrated in FIG. 3 , and a roller guide rail 1 a is formed below a door guide frame 1 corresponding to a window frame below the sliding window 4 so that the roller 4 r below the sliding window 4 slides on the roller guide rail 1 a while supporting the weight of the sliding window 4 . In addition, a downwardly opened upper pocket guide 1 d is formed on an upper portion 1 b of the door guide frame 1 corresponding to the window frame along the rail travel direction so as to guide the sliding of both the inner and outer surfaces (front and rear surfaces/inner and outer surfaces) of the upper end of the sliding window 4 in a state where the upper end of the sliding window 4 is accommodated inside of the upper pocket guide 1 d , thereby supporting the smooth movement of the sliding window above the sliding window 4 .
[0005] However, in view of the lower support structure on which the glass panel 4 g , the roller 4 r below the glass panel 4 g , and the roller guide rail 1 a below the roller 4 r are continuously supported when the sliding window 4 is made only using the glass panel 4 g without a door sash as described above, when a wind pressure W acts from the outside of the window as illustrated in the right side of FIG. 3 , the glass panel 4 g constituting the sliding window 4 and the upper pocket guide 1 d provided in a pocket shape in the upper portion 1 b of the door guide frame 1 has a structure capable of supporting the sliding window 4 even if the wind pressure W acts on the glass panel 4 g , but no separate structure capable of resisting against a transverse force such as the wind pressure W is provided among the glass panel 4 g constituting the sliding window 4 , the roller 4 r below the glass panel 4 g , and the roller guide rail 1 a . Therefore, the roller 4 r and the lower portion of the glass panel 4 g may be overturned (fall down) to a side of the window by the wind pressure.
[0006] As a method of solving such a problem, the lower structure of the door guide frame 1 forming the window frame may be improved to provide, on the lower portion of the door guide frame 1 , a lower pocket guide 1 c having a shape symmetric to the pocket-shaped upper pocket guide 1 d formed on the upper portion 1 b of the door guide frame 1 . That is, as illustrated in FIG. 4 , when an upwardly opened lower pocket guide 1 c is provided along the rail travel direction so as to guide the sliding of the lower end of the glass panel constituting the sliding window 4 on the both inner and outer surfaces (front and rear surface/inner and outer surfaces) of the window, the lower pocket guide 1 c may prevent the rotated (overturned) displacement of the lower end of the glass panel 4 g from exceeding a predetermined range even if a strong wind pressure is applied, which may cause the lower end of the glass panel 4 g and the roller 4 r supporting the glass panel 4 g to be overturned on the roller guide rail 1 a . As a result, a restoring force, which causes the lower end of the glass panel 4 g and the roller 4 r supporting the glass panel 4 g to maintain the vertical state again by the self-weight of the glass panel 4 g , acts so as to raise the roller 4 r up to a correct posture again so that the roller 4 r may return to the original position thereof.
[0007] Meanwhile, FIG. 4 illustrates the state where a location where the bottom surface of the lower end of the glass panel 4 g and the top surface of the upper end of the roller 4 r does not pass over a vertical center line C.L. of the roller guide rail 1 a which supports the roller 4 r (when a positive pressure and a negative pressure are equal to each other, the portions indicated by reference numerals “d 1 ” and “d 2 ” in FIG. 4 may be set to be equal to each other but according to a pressure condition, the portions indicated by reference numerals “d 1 ” and “d 2 ” may be set to be different from each other). Unlike this, however, when excessive overturn is caused so that a location, where the bottom surface of the lower end of the glass panel 4 g and the top surface of the upper end of the roller 4 r come in contact with each other to support the glass panel 4 g (the location indicated by reference numeral “k 1 ” in FIG. 4 ), passes over the vertical center line C.L. of the lower roller guide rail 1 a , it is impossible to expect the above-described restoring action. In such a case, the sliding window 4 is slid in the state where the glass panel 4 g and one side surface of the lower pocket guide 1 c are in contact with each other, thereby generating frictional noise as well as seriously damaging mobility.
[0008] Accordingly, the range of the width of the opening of the lower pocket guide 1 c should be set such that, even if the lower end of the glass panel 4 g and the roller 4 r are overturned, the location, where the bottom surface of the lower end of the glass panel 4 g and the top surface of the upper end of the roller 4 r are in contact with each other to the glass panel 4 g (reference numeral “k 1 ” in FIG. 4 ), does not pass over the vertical center line C.L. of the lower roller guide rail 1 a.
[0009] In addition, it may be assumed that the location, where the location where the bottom surface of the lower end of the glass panel 4 g and the top surface of the upper end of the roller 4 r are in contact with each other to support the glass panel 4 g as illustrated in FIG. 4 (reference numeral “k 1 ” in FIG. 4 ), is slid on the top surface of the upper end of the roller 4 r by itself. When such a phenomenon occurs, it is impossible to expect a satisfactory turnover prevention effect only by controlling the width of the opening of the lower pocket guide 1 c as described above. Thus, as illustrated in FIG. 5 , it may be preferable to provide a glass panel's lower end supporting shoulder 4 c on the upper end of the support bracket of the roller 4 r so as to prevent the slipping of the location where the bottom surface of the lower end of the glass panel 4 g and the top surface of the upper end of the roller 4 r are in contact with each other to support the glass panel 4 g (reference numeral “k 2 ” in FIG. 5 .
[0010] The sliding window with the above-described structure may stably support the sliding of the glass panel and roller while preventing the overturn of the glass panel and the roller in relation to a predetermined level of wind pressure. However, when the sliding window is enlarged as illustrated in FIG. 6 which illustrates a front view of a sliding window system and FIG. 7 which illustrates a cross-section taken along line A-A′ in FIG. 6 , the vertical length (height) of the glass panel 4 g increases so that a critical situation may occur in enduring the transverse bending deformation of the glass panel 4 g only with the rigidity of the glass panel 4 g under a strong wind pressure condition, and the transverse bending deformation with reference to the vertical line of the glass panel 4 g may exceed a yield point of the glass panel 4 g due to the strong wind (wind pressure). In such a case, there is a strong likelihood that the glass panel may be destroyed.
[0011] In order to solve this problem, as illustrated in FIG. 8 , an improved structure may be preferably adopted which is provided with an additional means capable of controlling the transverse bending deformation of a glass panel 41 by configuring a sliding window 40 including the glass panel 41 supported by a roller 43 and rigidly joining a separate vertical stiffener 42 to a side surface of the glass panel. The vertical stiffener 42 is provided to exhibit high rigidity as compared to a case where only the glass panel 4 g is provided as described above. Most preferably, when a stiffener 42 made of a material which may exhibit high bending rigidity with the same thickness as that of the glass panel 41 is rigidly joined to the side surface of the glass panel 41 , it may be of help to simplify the lower support structure. Due to a limit in rigidity of raw materials of conventionally used construction materials, however, the vertical stiffener 42 will have a structure, of which the thickness b 1 is thicker than the thickness b 1 of the glass panel 41 as illustrated in FIG. 8 . Meanwhile, the lower end of the vertical stiffener 42 is formed as a stiffener's narrow end 42 a , of which the thickness b 4 is reduced such that it may be inserted into the width b 2 of the opening of the lower pocket guide 13 provided in the lower door guide frame 10 including the roller guide rail 11 that supports the roller 43 of the sliding window 40 . Further, the upper end of the vertical stiffener 42 should also be formed as a stiffener's narrow end of which the thickness b 4 is reduced such that it may be inserted into the width of the opening of the upper pocket guide 14 provided to be downwardly opened on the upper door guide frame 10 , which constitutes the window frame of the sliding window 40 . In such a case, as illustrated in the cross-sectional view of FIG. 9 , the smooth movement of the sliding window 40 may be ensured when predetermined separation distances (reference numerals e and e′ in FIG. 9 ) are secured between the heights of the thickness-reduced stiffener's narrow-ends 42 a and the heights of the lower pocket guide 13 and the upper pocket guide 14 which are provided in the lower and upper portions of the door guide frame 10 , respectively. However, when the separation distances e and e′ increase, the resistance against the wind pressure is weakened.
[0012] In addition, when the thickness b 3 of the vertical stiffeners 42 is larger than the width b 2 of the openings of the lower pocket guide 13 and the upper pocket guide 14 , the thickness b 4 of the stiffener's narrow-ends 42 a should be reduced to be capable of being inserted into the width b 2 of the openings of the lower and upper lower pocket guides 13 and 14 .
[0013] Of course, even in such a case, another requirement that the minimum value Min (e′, g′) (denoted by reference numeral h in FIG. 10 ) between the separation distance e′ between the lower end of the upper stiffener's narrow end 42 of the sliding window 40 and the outer lower end of the upper pocket guide 14 provided in the upper portion of the door guide frame 10 and the spacing distance g′ between the inner upper end of the upper pocket guide 14 and the upper end of the sliding window 40 should be larger than the depth of the glass panel 41 (denoted by reference numeral f in FIG. 12 ) inserted into the lower pocket guide 13 (h=Min(e′, g′)>f) should be satisfied so that, so that when the sliding window 40 is lifted upward as illustrated in FIG. 10 , the lower end of the stiffener narrow-end 42 a may be released from the opening of the lower pocket guide 13 as illustrated in FIG. 11 so as to enable installation/removal of the sliding window 40 in the state where the vertical stiffeners 42 are integrated with the glass panel 41 . However, here, in order to secure a sufficient upward displacement which may be obtained when the sliding window 40 is fully lifted, it may be preferable to provide a structure in which the separation distance e′ between the lower end of the upper stiffener's narrow end 42 a of the sliding window 40 and the outer lower end of the upper pocket guide 14 provided in the upper portion of the door guide frame 10 is set to be larger than the separation distance g′ between the inner upper end of the upper pocket guide 14 and the upper end of the sliding window 40 .
[0014] Whereas, as illustrated in FIG. 12 , when the minimum value Min (e′, g′) (denoted by reference numeral h in FIG. 10 ) between the separation distance e′ between the lower end of the upper stiffener's narrow end 42 of the sliding window 40 and the outer lower end of the upper pocket guide 14 provided in the upper portion of the door guide frame 10 and the spacing distance g′ between the inner upper end of the upper pocket guide 14 and the upper end of the sliding window 40 is smaller than the depth of the glass panel 41 (denoted by reference numeral f in FIG. 12 ) inserted into the lower pocket guide 13 (h=Min(e′, g′)<f), it is impossible to secure an upward displacement which may be obtained when the sliding window 40 is fully lifted so that the lower end of the stiffener narrow-end 42 a cannot be released from the opening of the lower pocket guide 13 due to interference of an upper end protrusion of the lower pocket guide 13 . Thus, the sliding window 40 cannot be installed/removed merely by lifting and rotating the sliding window 40 so that the lower end is released from the lower pocket guide 13 . Up to now, the removal/installation by lifting the sliding window 40 has been described with reference to FIGS. 9 to 11 . On the contrary, a requirement of enabling the installation/removal of the sliding window 40 and a requirement of disabling the installation/removal of the sliding window 40 exist separately in the method of rotating the upper end of the sliding window 40 in the state where the roller 43 below the sliding window 40 is removed from sliding window 40 and lowering the sliding window 40 so as to cause the upper end of the sliding window 40 to be released from the upper pocket guide 14 . However, since this is symmetrically similar to the above-described case, redundant descriptions will be omitted. However, a person ordinarily skilled in the art may easily understand and conceive the contents omitted due to the redundancy.
[0015] As described above, a case corresponding to the requirement of disabling the removal/installation in relation to the door guide frame 10 of the sliding window 40 formed by rigidly joining the vertical stiffeners 42 to a side surface of the glass panel 41 may occur. In such a case, as illustrated in FIG. 12 , an inconvenience may occur in that the vertical stiffeners 42 should be joined to the glass panel 41 through an on-site installation method after the glass panel 41 is installed by inserting the glass panel 41 into the upper pocket guide 14 and the lower pocket guide 13 . Once the installation is completed, the sliding window 40 cannot be separated from the door guide frame 10 unless the vertical stiffeners 42 are separated from the glass panel 41 again or the glass panel 41 is damaged.
[0016] In order to enable the factory production of the sliding window 40 provided with the vertical stiffeners 42 without causing inconvenience in the on-side installation of the vertical stiffeners 42 , and after the installation, to avoid the problem that makes the separation of the sliding window 40 including the vertical stiffeners 42 impossible, a sufficient separation distance e should be secured between the upper end of the stiffener's narrow end 42 a and the upper end of the lower pocket guide 13 provided in the lower portion of the door guide frame 10 . However, in such a case, structural instability in relation to the wind pressure is caused due to the excessive separation distance e and there is a considerable disadvantage in hermeticity.
[0017] In addition, the installation structure of the ordinary sliding window in the prior art has a conventional installation structure in which the lower door guide frame that constitutes the window frame supporting the sliding window is installed on a floor surface of a building after the floor surface is constructed. However, such an installation structure also has a problem in that the door guide frame and the roller guide rail included therein protrude upward from the floor surface, thereby detracting from the beauty and serving as an obstacle in relation to a pedestrian or a moving object crossing them. As a result, installation of the sliding door itself may be abandoned in some cases.
[0018] In addition, when construction is performed such that a portion connecting an indoor area inside of a building and an outdoor terrace is entirely opened and a window is installed therein, a folding door or the like is frequently installed since it is difficult to implement a large sliding window by using a sliding door roller and a support structure thereof according to the prior art is used. However, the folding door has a problem in that since the folding door requires a folding space, the availability of the building floor surface deteriorates.
DETAILED DESCRIPTION OF THE INVENTION
Technical Problem
[0019] The present invention has been made in order to solve the problems in the prior art and a technical object of the present invention is to provide a structure adopted for supporting a smooth movement of a sliding window, in which a glass panel forming the sliding window which constitutes a sliding window system is directly placed on and supported by a roller member without a separate quadrilateral door sash that supports the glass panel forming the sliding window so as to minimize a phenomenon of reducing the open view through the sliding window that constitutes the sliding window system, and upper and lower pocket guides are respectively formed in upper and lower door guide frames used as window frame members that guide a sliding movement of the sliding window so that the upper and lower pocket guides guide the upper end and lower end of the sliding window in both inner and outer surfaces (front and rear surfaces/inner and outer surfaces) of the sliding window, characterized in that factory production of the sliding window provided with vertical stiffeners may be technically allowed by rigidly joining the vertical stiffeners having an enlarged cross-section (having a thickness larger than that of the glass panel) to both side surfaces of the glass panel that constitutes the sliding window including the glass panel supported by the roller so as to reinforce the transverse bending rigidity of the glass panel, and configuring the sliding window provided with the vertical stiffeners to be integrally installed within the door guide frame, and the sliding window provided with the vertical stiffeners may be separated even after the installation of the sliding window.
[0020] In addition, the present invention is to provide a technical means capable of improving water-tightness, air-tightness, and heat insulation as well, in achieving the above-described technical object.
[0021] Further, another technical object of the present invention is to provide a sliding window installation structure in which a door guide frame and a roller guide frame do not protrude above a floor surface of a building when a structure in which a lower portion of a window frame is positioned on a floor surface of a building so as to secure a wider open view is adopted as the sliding window installation structure.
Technical Solution
[0022] In order to solve the above-described problems, the present invention provides a sliding window installation structure including a door guide frame of a separable and removable segment structure, in which a glass panel forming the sliding window (e.g., a pair glass) constituting a sliding window system is removably seated on and supported by rollers without a separate quadrilateral door sash that supports the glass panel forming the sliding window so as to minimize a phenomenon of reducing an open view through the sliding window, and upper and lower pocket guides are respectively formed in upper and lower door guide frames used as a window frame member that guides a sliding movement of the sliding window so as to guide the upper end and lower end of the sliding window in both inner and outer surfaces (front and rear surfaces/inner and outer surfaces) of the sliding window, thereby supporting a smooth movement of the sliding window.
[0023] Vertical stiffeners with an enlarged cross-section (cross-section having a thickness thicker than the glass panel) may be attached to both side surfaces of the glass panel that constitutes the sliding window including the glass panel supported by the rollers so as to reinforce transverse bending rigidity of the glass panel.
[0024] In order to allow the sliding window provided with the vertical stiffeners to be integrally installed within a door guide frame, and to allow the sliding window to be separated from the door guide frame in a state where the sliding window is provided with the vertical stiffeners, a pocket guide configured to guide and support a stiffener's narrow end formed at an end of each vertical stiffener to have a reduced cross-sectional thickness on both inner and outer surfaces of the sliding window is installed to be separable from a door guide frame body in a direction parallel to the travel direction of a roller guide rail installed on a base surface of the door guide frame body including an opening having a size larger than the cross-sectional thickness of the vertical stiffener. The pocket guide is formed by pocket guide segments removable from the door guide frame body, and the pocket guide segments are successively installed to be separable from each other on both the inner and outer surfaces of the sliding window along the travel direction of the roller guide rail.
[0025] The pocket guide segments provided as the pocket guide may be provided in at least one of an upper structure and a lower structure of the door guide frame, when the pocket guide segments are both the upper and lower structures of the door guide frame, so that the sliding window may be variously installed and removed.
[0026] Here, the pocket guide segments provided as the pocket guides inside and outside of the sliding window may be divisionally formed as two or more segments over the entire length of the roller guide rail, and one or more segments may be formed to have a length removable from the door guide frame body in a state where the sliding window is installed to be seated on the rollers on the roller guide rail. In addition, the length of the pocket guide segments may be determined to be smaller than an inner gap between the vertical stiffeners attached to the both sides of the sliding window.
[0027] In order to improve dust resistance (dust inflow prevention capability), water-tightness, and air-tightness of the sliding window system having the above-described structure, blocking members such as mohairs or elastic gaskets may be installed in a horizontal longitudinal direction on opposite surfaces of the pocket guide segments provided as the pocket guides and the sliding window. More preferably, each of the elastic gaskets provided as the blocking members may include a fixed end fixed to the sliding window and an elastically deformable end which is in contact with an opened surface of the pocket guide segments provided as the pocket guides to be deformed outwardly.
[0028] In order to improve window openness and heat insulation, a vertical stiffener insertion channel may be provided inside of the vertical guide frame forming the door guide frame so that the vertical stiffener constituting the sliding window is inserted into and concealed when the sliding window is closed, and a vertical elastic gasket may be provided in an end of the vertical guide frame provided with the vertical stiffener insertion channel to hermetically block a gap between the vertical guide frame and the vertical stiffener.
[0029] Further, the lower structure of the door guide frame, in which the pocket guide segments are removably installed in the door guide frame body, may be embedded in a floor surface of a building.
Advantageous Effects
[0030] According to the present invention, since the glass panel forming the sliding window constituting the sliding window system is directly mounted on the roller member to be supported without a separate quadrilateral door sash that supports the glass panel forming the sliding window, a phenomenon of reducing an open view through the sliding window can be minimized. Since the vertical stiffeners having an enlarged cross-section (cross-section having a thickness thicker than the glass panel) are rigidly joined to the opposite side surfaces of the glass panel supported by the roller, the transverse bending rigidity of the glass panel can be reinforced to exhibit high wind pressure resistance. Further, the sliding window is configured to be installed inside of the door guide frame to be integrally installed in a state in which the sliding window is provided with the vertical stiffeners, so that the sliding window can be directly manufactured in a factory. Moreover, the sliding window having an enlarged cross-section by being provided with the vertical stiffeners can be removed from the door guide frame even after installation without any interference.
[0031] In addition, the sliding window system according to the present invention may also improve water-tightness, air-tightness, and heat insulation.
[0032] Further, according to the present invention, the door guide frame serving as the lower structure of the window frame is configured to be positioned under a floor surface of a building so as to secure a wider open view in the sliding window installation structure. Thus, it is possible to provide a sliding window installation structure in which the door guide frame and the roller guide rail do not protrude above the floor surface of the building.
BRIEF DESCRIPTION OF THE DRAWINGS
[0033] FIGS. 1 and 2 are views illustrating a conventional sliding window system which is provided with a door sash which supports a glass panel on the four sides of the glass panel.
[0034] FIGS. 3 to 5 are views illustrating a sliding window installation structure which improves the conventional sliding window system of FIGS. 1 and 2 by directly mounting a glass panel on a roller without a door sash to be used as a sliding window.
[0035] FIGS. 6 and 7 are schematic views for illustrating a problem of reducing wind pressure resistance due to lack of rigidity of the glass panel of the improved sliding window illustrated in FIGS. 3 to 5 , and FIG. 8 is a view illustrating a state in which a vertical stiffener is attached to a side surface of the glass panel which constitutes the sliding window in order to solve the problem.
[0036] FIGS. 9 to 13 are schematic views for describing problems caused when installing and removing the single window in which the problems are additionally caused in the improved sliding window illustrated in FIG. 8 due to the addition of the vertical stiffeners.
[0037] FIG. 14 is a cross-sectional view illustrating a sliding window installation structure according to the present invention.
[0038] FIGS. 15 to 17 are cross-sectional views illustrating a sliding window installation structure in according to a first embodiment of the present invention which conventional axial type rollers are used, and an operating state thereof.
[0039] FIGS. 18 to 21 are views illustrating a sliding window installation structure according to a second embodiment of the present invention in which annular roller devices are used for a sliding window, and an operating state thereof.
[0040] FIGS. 22 to 27 are plan views illustrating in sequence a process of removing pocket guide segments from a door guide frame body and removing a sliding window provided with a vertical stiffener from a window frame in a sliding window installation structure according to the present invention.
[0041] FIG. 28 is a plan view illustrating an operating state of an embodiment using pocket guide segments divided unlike the embodiment illustrated in FIGS. 22 to 27 .
[0042] FIG. 29 is a plan view illustrating a plan view for describing an additional characteristic structure for improving heat insulation in the sliding window installation structure according to the present invention and an effect thereof, and FIG. 30 is a plan view illustrating a comparative embodiment from which the characteristic structure is removed.
[0043] FIG. 31 is a view illustrating a preferable width of an opening between lower pocket guides according to the present invention.
[0044] FIG. 32 illustrating an embodiment of the present invention in which support shoulders for supporting a lower end of a glass panel are formed on the upper end of a roller support bracket.
[0045] FIGS. 33 and 34 are perspective views illustrating an embodiment of the present invention to which the sliding window installation structure of the present invention is applied to an aluminum window frame system.
[0046] FIG. 35 is a view illustrating an embodiment in which a steel reinforcement plate in an insert form is inserted into a vertical stiffener.
[0047] FIGS. 36 and 37 are views for describing an embodiment in which a lower structure of a door guide frame, in which pocket guide segments according to the present invention are removably installed in a door guide frame body, is embedded in a floor surface of a building.
MODE FOR CARRYING OUT THE INVENTION
[0048] Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings such that a person ordinarily skilled in the art to which the present invention belongs may easily embody the present invention. However, the present invention may be implemented in various forms and is not limited to the embodiments described herein.
[0049] As described above, the present invention is intended to solve a problem of weakening wind pressure resistance due to lack of rigidity of a sliding window improved to enhance openness of a window as described above as well as a problem caused when installing/removing the sliding window simultaneously. FIG. 14 is a cross-sectional view illustrating a sliding window installation structure according to the present invention
[0050] FIGS. 15 to 17 are cross-sectional views illustrating a sliding window installation structure according to a first embodiment of the present invention in which conventional axial type rollers are used, and an operating state thereof.
[0051] An embodiment of the present invention exemplified in the drawings provides a sliding window installation structure for supporting a smooth movement of a sliding window 400 , in which a glass panel (e.g., a pair glass) 410 forming the sliding window 410 which constitutes a sliding window system is directly placed on and supported by rollers 450 without a separate quadrilateral door sash that supports the glass panel 410 forming the sliding window 400 so as to minimize a phenomenon of reducing an open view through the sliding window 400 , and upper and lower pocket guides 130 are respectively formed in upper and lower door guide frames 100 used as window frame members that guide a sliding movement of the sliding window so that the upper and lower pocket guides 130 guide the upper end and lower end of the sliding window in both inner and outer surfaces (front and rear surfaces/inner and outer surfaces) of the sliding window 400 .
[0052] Vertical stiffeners 420 , each of which has an enlarged cross-section (having a thickness larger than that of the glass panel), are attached to both side surfaces of the glass panel 410 that constitutes the sliding window 400 including the glass panel 410 supported by the rollers 450 so as to reinforce the transverse bending rigidity of the glass panel 410 .
[0053] In order to allow the sliding window 400 provided with the vertical stiffeners 420 to be integrally installed within a door guide frame 100 , and to allow the sliding window 400 to be separated from the door guide frame 100 in a state where the sliding window 400 is provided with the vertical stiffeners 420 , the sliding window installation structure includes: a door guide frame with a separable and removable segment structure, in which a pocket guide 130 configured to guide and support a stiffener's narrow end 420 a formed at an end of each vertical stiffener 420 to have a reduced cross-sectional thickness on both inner and outer surfaces (front and rear surfaces/inner and outer surfaces) of the sliding window 400 is installed to be separable from a door guide frame body 120 in a direction parallel to the travel direction of a roller guide rail 110 installed on a base surface 121 of the door guide frame body 120 including an opening having a size larger than the cross-sectional thickness of the vertical stiffener 420 , in which the pocket guide 130 is formed by pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) (see FIGS. 22 to 27 ) removable from the door guide frame body 120 , and the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) are successively installed to be separable from each other on both inner and outer surfaces of the sliding window 400 along the travel direction of the roller guide rail 110 .
[0054] Here, in order to removably install the pocket guide 130 on the base surface 121 of the door guide frame body 120 , as illustrated in FIG. 14 , partition walls 122 are formed outside of the base surface 121 to protrude along the travel direction of the roller guide rail 110 , in which the roller guide rail 110 is provided at a central portion of the base surface 121 , so that accommodation portions 123 may be formed between outer walls of the door guide frame body 120 and the partition walls 122 so as to install the pocket guide 130 by inserting the pocket guide 130 into the accommodation portions 123 .
[0055] In addition, the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guide 130 may be provided in an upper structure and/or a lower structure of the door guide frame 100 (in the state illustrated in FIG. 14 , the pocket guide segments are provided only in the lower structure). When the pocket segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) are provided in both the upper structure and the lower structure of the door guide frame 100 as illustrated in FIGS. 15 to 17 , the sliding window 400 may be installed/removed in various directions.
[0056] Upon comparing the first embodiment illustrated in FIGS. 15 to 17 with the basic structure illustrated in FIG. 14 , the shapes of the pocket guide segments ( 130 : 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides 130 at both structures and the shapes of the accommodation portions 123 in which the pocket guides 130 may be installed by being inserted are differently illustrated in the drawings. However, although the functional principles of both structures are substantially equal to each other, the first embodiment further improves the structural stability.
[0057] According to the sliding window installation structure including the door guide frame with the separable and removable segment structure as described above, when the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guide 130 in one of the upper structure and the lower structure of the door guide frame 100 as illustrated in FIGS. 16 and 17 are removed from the door guide frame 100 , the sliding window 400 may be easily separated from the door guide frame 100 even if the sliding window 400 is provided with the vertical stiffeners 420 . On the contrary, the sliding window 400 may be easily assembled to and installed in the door guide frame 100 in the state where the vertical stiffeners 420 are integrated through a production process in a factory or the like. In addition, as illustrated in FIG. 15 , the separation distance e′ between the lower end of the stiffener's narrow end 420 a in the upper portion of the sliding window 400 and the outer lower end of the upper pocket guide 130 provided in the upper portion of the door guide frame 100 , and the separation distance e between the upper end of the stiffener's narrow end 420 a in the lower portion of the sliding window 40 and the outer upper end of the upper pocket guide 130 provided in the upper portion of the door guide frame 100 can be minimized, and a structure capable of maximizing the wind pressure resistance and the hermeticity can be achieved.
[0058] FIGS. 18 to 21 are views illustrating a sliding window installation structure according to a second embodiment of the present invention in which annular roller devices are used for a sliding window, and an operating state thereof. The second embodiment illustrated in FIGS. 18 to 21 uses annular roller devices 500 specially designed to smoothly support and move a heavy sliding window even if the annular roller devices 500 have a small size, instead of the conventional rollers 450 described above.
[0059] In addition, in order to improve dust resistance, water-tightness, and air-tightness of the sliding window system having the above-described structure, as illustrated in FIGS. 18 and 19 , blocking members such as mohairs 131 or elastic gaskets 431 may be installed in a horizontal longitudinal direction on the opposite surfaces of the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides 130 and the sliding window 400 .
[0060] Here, as illustrated in FIGS. 18 and 19 , each of the elastic gaskets 431 provided as the blocking members including a fixed end fixed to the sliding window 400 and an elastically deformable end which is in contact with an opened surface (in the drawings, the top surface in the case of the lower structure/the lower surface in the case of the upper structure) of the pocket guide segments ( 130 : 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides 130 to be deformed outwardly may be more preferably used from the view point of blocking inflow of rain. Unlike this, when the elastically deformable end of the elastic gasket 431 is in contact with an inner closed surface of the pocket guide segments ( 130 : 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides 130 to be elastically deformed inwardly as in the case of comparative example A comparatively illustrated in the lower portion of FIG. 18 , the elastically deformable end is sandwiched between the sliding window 400 and a pocket guide segment 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) so that the smooth sliding movement of the sliding window 400 may be hindered due to the friction of the elastically deformable end and the inflow of rain may not be efficiently blocked.
[0061] Meanwhile, as illustrated in FIGS. 18 and 19 , it is preferable that the elastic gaskets 431 are installed on glass support stages 430 coupled to the lower ends of the glass panels 410 which form a pair glass.
[0062] Hereinbelow, a configuration and action of annular roller devices 500 used in the second embodiment will be described with reference to FIGS. 20 and 21 .
[0063] According to the second embodiment of the present invention, an annular roller device 500 is used as the roller member that supports the sliding window 400 below the sliding window 400 and allows the sliding window 400 to be slid along the roller guide rail 110 as illustrated in FIGS. 20 and 21 . The annular roller device 500 includes: a glass seat 510 formed by a support bracket on a top central portion to be capable of accommodating a lower end of the glass panel 410 (in FIGS. 18 and 19 , a glass support stage 430 ) that constitutes the sliding window 400 ; weight support plates 520 formed integrally by extending partition walls formed downwardly at opposite sides of the glass seat 510 from the glass seat 510 and including a guide rail 525 formed along the rail travel direction around the weight support plates 520 ; a plurality of rolling members 532 , each of which is formed in a cylindrical shape laid in a transverse direction to be orthogonal to the rail travel direction and includes a guide recess 532 a formed on the outer circumferential surface thereof along the rail travel direction; and a plurality of chain link units 534 configured to interconnect the plurality of rolling members 532 such that the plurality of rolling members 532 are evenly disposed in an annular shape on a surface of the weight support plate 520 to be spaced by a preset interval along a door travel direction. The annular roller device 500 further includes an annular rolling unit 530 wound around the top surface and the bottom surface of the weight support plates of the opposite sides of the glass seat 510 and circular arc surfaces formed in the rail travel direction at the opposite ends to interconnect the top surface and the bottom surface.
[0064] Here, the weight support plates 520 formed at the opposite sides of the glass seat 510 have a flat plate shape and evenly support the weight of the sliding window 400 while serving as a rotation shaft of the annular rolling units 530 , and the opposite ends of the weight support plates 520 are formed preferably in a circular arc shape so that the plurality of rolling members 532 may be smoothly rotated on the opposite ends of the weight support plates 520 . Since the weight support plates 520 have the flat plate shape unlike the conventional roller device having a cylindrical shape formed with a central bore (see FIG. 5 ), the entire height may be considerably reduced in transferring and supporting a weight through a wide area. Consequently, the weight support plates 520 may be installed even if the height of an installation height is low.
[0065] The annular rolling unit 530 having a configuration as illustrated in FIGS. 20 and 21 are wound around the weight support plates 520 at the opposite sides of the glass seat 510 to rotate around the weight support plates 520 as an axis. specifically, the annular rolling unit 530 includes a plurality of rolling members 532 , and a plurality of link units 534 configured to interconnect the plurality of rolling members 532 such that the plurality of rolling members 532 may be spaced apart from each other at a preset interval and evenly distributed on the surfaces of the weight support plates 520 , i.e. the top surface, the bottom surface, and the opposite circular arc shapes. Thus, the length of the annular rolling unit 530 may be adjusted to be suitable for the length of the weight support plate by adjusting the number of the rolling members 532 and the length of the link units 534 . Further, unlike a conventional roller device having a construction in which the weight of the sliding window 400 is completely concentrated to linear contact surfaces of bearing parts, in the present invention, the plurality of rolling members 532 may support the weight of the sliding window 400 while evenly distributing the weight of the sliding window 400 so that the sliding window 400 which is heavy as compared to the conventional one can be supported. In addition, each of the plurality of rolling members 532 may be made of a self-lubricating material. When the self-lubrication material is used, a lubricant material such as oil may not be separately used so that the costs may be reduced and surroundings may be kept clean.
[0066] Meanwhile, a process of assembling the annular rolling unit 530 and the weight support plates 520 will be described with reference to FIG. 21 . A corresponding external link members 534 of the annular rolling unit 530 is separated, then the annular rolling unit 530 is wound on the weight support plates 120 such that the guide rails 525 of the weight support plates 520 and the guide recesses 532 a of the plurality of rolling members 532 correspond to each other, and then the corresponding external link members 534 are fastened. Then, the assembly of the annular rolling unit 530 is completed.
[0067] In the case of the annular rolling unit 530 assembled as described above, the guide recesses 532 a of the plurality of rolling members 532 and the guide rails 525 of the weight support plates 520 are correspondingly engaged with each other, and as illustrated in the lower portion of FIG. 20 in an enlarged scale, the guide recesses 532 a are also correspondingly engaged with a guide rib 111 of the roller guide rail 110 installed on the base surface 121 of the door guide frame body 120 in the lower structure of the door guide frame 100 , so that the annular rolling unit 530 may be smoothly slid while rotating around the weight support plates 520 to maintain the straight travel property of the sliding window 400 .
[0068] With the annular roller device 500 , even if the weight support plates 520 are tilted left and right, tilting of the annular rolling unit 530 to one side (i.e., a phenomenon hindering the smooth straight travel of the sliding window) may be prevented in advance, and slippage of the annular rolling unit 530 to the left or right side of the weight support plates 520 during the annular rolling unit 530 may also be prevented in advance. As such, since the external link members 534 may be prevented from rubbing against the door guide frame 100 in advance, cutting of the annular rolling unit 530 caused by the wear and tear of the external link members 534 may be prevented in advance.
[0069] In the case of the sliding window systems according to the embodiments described above, descriptions will be made on the configuration which allows the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides ( 130 ) to be easily separated from the body 120 of the door guide frame 100 without interfering with the sliding window 400 , and the operating procedure thereof.
[0070] First, as illustrated in FIGS. 22 to 30 , the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) provided as the pocket guides 130 inside and outside of the sliding window 400 are divisionally formed as two or more segments over the entire length of the roller guide rail 110 , and one or more segments may be formed to have a length removable from the door guide frame body 120 in a state where the sliding window 400 are installed to be seated on the rollers 450 on the roller guide rail 110 . In addition, the length of the pocket guide segments 130 ( 130 {circle around ( a )}, 130 {circle around ( b )}, or 130 {circle around ( c )}) may be determined to be smaller than an inner gap between the vertical stiffeners 420 attached to the both sides of the sliding window 400 .
[0071] Hereinafter, the operation of the present invention will be described with reference to FIGS. 22 to 27 , assuming that three pocket guide segments 130 {circle around ( a )}, 130 {circle around ( b )} and 130 {circle around ( c )} are divisionally installed as the pocket guides 130 inside and outside of the sliding window 400 along the entire length of the roller guide rail 110 , as an example.
[0072] First, when the sliding window 400 is in the closed state as illustrated in FIG. 22 , the sliding window 400 is in the state where it cannot be easily removed from the door guide frame 100 due to the interference between the pocket guide segments 130 {circle around ( a )} and 130 {circle around ( b )} provided as the pocket guides 130 . However, the segment 130 {circle around ( c )} located at a position where the sliding window 400 is not positioned as illustrated in FIG. 23 may be removed from the body 120 of the door guide frame 100 . Then, when the sliding window 400 is slid to be partially opened as illustrated in FIG. 24 so that the sliding window 400 is positioned on the intermediate pocket guide segment 130 {circle around ( b )}, since the pocket guide segment 130 {circle around ( b )} has a length shorter than the interval between vertical stiffeners 420 positioned on the opposite side surfaces of the sliding window 400 , the intermediate pocket guide segment 130 {circle around ( b )} may also be removed from the body 120 of the door guide frame 100 without interference with the sliding window 400 as illustrated in FIG. 25 . In the state illustrated in FIG. 26 in which two pocket guide segments 130 {circle around ( c )} and 130 {circle around ( b )} are removed from the body 120 of the door guide frame 100 , the sliding window 400 may be removed from the door guide frame 100 without interference from the body 120 of the door guide frame 100 as described above with reference to FIGS. 16 , 17 and 19 . The state in which the sliding window 400 is removed is illustrated in FIG. 27 .
[0073] Meanwhile, the order performed from FIGS. 22 to 27 may be referred to as the steps of removing the sliding window 400 from the door guide frame 100 and on the contrary, the order performed from FIG. 27 to FIG. 22 may be referred to as the steps of installing the sliding window 400 in the door guide frame 100 .
[0074] The embodiment described above exemplifies a case in which three pocket guide segments 130 {circle around ( a )}, 130 {circle around ( b )} and 130 {circle around ( c )} are divisionally installed as the pocket guide 130 inside and outside of the sliding window 400 along the entire length of the roller guide rail 110 . Unlike this, descriptions will be made in terms of removal and installation of a front sliding window assuming that a window denoted by reference numeral 200 in FIG. 28 is a fixed window having a width which is larger than the front sliding window 400 . In this case, it can be seen that the present invention may be implemented by divisionally installing the pocket guide segments 130 {circle around ( a )} and 130 {circle around ( b )} having different lengths as the pocket guides 130 . That is, in this case, the pocket guide segment 130 {circle around ( b )} larger than the entire width of the sliding window 400 may be removed from the door guide frame 100 so that the sliding window 400 may be removed from the door guide frame 100 or installed in the door guide frame 100 without any difficulty.
[0075] In addition, descriptions will be made on an additional embodiment in terms of improvements in window openness and heat insulation among the technical objects of the present invention with reference to FIGS. 29 and 30 . FIG. 29 is a plan view illustrating an additional characteristic structure for improving heat insulation in the sliding window installation structure according to the present invention, and FIG. 30 is a plan view illustrating a comparative example in which the characteristic structure is removed.
[0076] First, the comparative embodiment illustrated in FIG. 30 will be described. When the sliding window 400 is closed, the vertical stiffener 420 constituting the sliding window 400 is exposed to the outside without entering the inside of the vertical guide frame 101 forming the door guide frame 100 constituting the window frame. As a result, the complete openness is hindered by the vertical stiffener 420 , thereby disturbing an open view through the window, and heat insulation deteriorates.
[0077] On the contrary, in the additional embodiment of the present invention, when the sliding window 400 is closed, a vertical stiffener insertion channel 101 a is provided inside of the vertical guide frame 101 forming the door guide frame 100 as illustrated in FIG. 29 so that the vertical stiffener 420 constituting the sliding window 400 is inserted into and concealed by the vertical guide frame 101 forming the door guide frame 100 constituting the window frame. A vertical elastic gasket 101 s may be provided in the end of the vertical guide frame 101 provided with the vertical stiffener insertion channel 101 a to hermetically block a gap between the vertical guide frame 101 and the vertical stiffener 420 . With this structure, the vertical stiffener 420 is concealed not to hinder the complete openness of the window while improving heat insulation.
[0078] However, the vertical stiffener insertion channel 101 a may be opened to the inside of the vertical guide frame 101 when configuring the sliding window system according to design requirements such as a position on a plane, the direction of closing the sliding window, the sizes of the sliding window and the window frame. Alternatively, some vertical stiffener insertion channels 101 a may be selectively closed in advance by a blocking block 150 which is separately manufactured and assembled by being inserted into the vertical stiffener insertion channel 101 a in the vertical direction.
[0079] Meanwhile, in the case of the lower pocket guides 130 according to the present invention, the width B 2 of the opening between the lower pocket guides 130 installed inside and outside of the window to be removable from the door guide frame body 120 should have a range determined such that, even if the lower end of the glass panel 410 provided with the vertical stiffener 420 and the roller 450 are turned over, the location (reference numeral “k 1 ” in FIG. 31 ), where the bottom surface of the lower end of the glass panel 410 and the top surface of the upper end of the roller 450 are in contact with each other to support the glass panel 410 , shall not pass over the vertical center line C.L. of the lower roller guide rail 110 .
[0080] In addition, it may be considered that the location (reference numeral “k 1 ” in FIG. 31 ), where the bottom surface of the lower end of the glass panel 410 and the top surface of the upper end of the roller 450 are in contact with each other to support the glass panel 410 as illustrated in FIG. 31 , is slid on the top surface of the upper end of the roller 450 . When such a phenomenon occurs, a satisfactory turnover prevention effect cannot be expected only with the above-described control of the width B 2 of the opening of the lower pocket guide 130 . Thus, in order to prevent the slippage of the location (reference numeral “k 2 ” in FIG. 32 ), where the bottom surface of the lower end of the glass panel 410 and the top surface of the upper end of the roller 450 are in contact with each other to support the glass panel 410 , support shoulders 451 a for supporting the lower end of the glass panel may be provided on the upper end of the support bracket 451 of the roller 450 as illustrated in FIG. 32 . The support shoulders 451 a supporting the lower end of the glass panel are also presented in the first embodiment illustrated in FIGS. 16 and 17 , and in the second example using the annular roller device 500 illustrated in FIGS. 18 to 21 , the glass seat 510 provided for the same purpose as the support bracket 451 may also be provided with support shoulders 510 a for supporting the lower end of the glass panel.
[0081] Meanwhile, the sliding window installation structure according to the present invention described up to now may be made of a synthetic resin such as PVC or an aluminum material. In particular, when the sliding window installation structure is made of the aluminum material, it will be more advantageous to adopt a structure in which the body 120 of the door guide frame 100 is formed to be divided into portions inside and outside of the window and a thermal break material 120 m is interposed therebetween. In addition, the pocket guide 130 may also be formed such that a region 130 m to be in contact with the thermal break material 120 m of the door guide frame body 120 is formed of the thermal break material in separation of the remaining cap region 103 c.
[0082] In addition, a rail installation recess 110 a may be formed on the base surface 121 of the door guide frame 100 such that the roller guide rail 110 manufactured according to the size and type of the roller (the conventional roller 450 in FIG. 33 or the annular roller device 500 in FIG. 34 ) may be inserted and installed to be replaceable.
[0083] In addition, when the synthetic resin such as PVC or aluminum is used as the material for the sliding window installation structure according to the present invention and the window is enlarged, the thickness of the vertical stiffeners 420 may be excessively thick due to the limit of rigidity of the material. In order to alleviate such a problem by providing high bending rigidity as compared to a cross-sectional size, a steel reinforcement plate 422 in an insert form may be inserted into the vertical stiffener 420 as illustrated in FIG. 35 .
[0084] Meanwhile, as an embodiment provided in another point of view of the present invention, a sliding window installation structure using a sliding window system provided with a door guide frame 100 which may be embedded in the floor surface of a window installation structure may be provided as illustrated in FIGS. 36 and 37 in which a door guide frame 100 , which is provided with removable pocket guides 130 divisionally installed as pocket guide segments, is embedded in a building floor surface 600 . According to this structure, the view openness of the sliding window may increase as illustrated in FIG. 36 . In addition, since the door guide frame 100 has a structure which does not protrude above the floor surface in the state where the pocket guide 130 constituting the upper structure of the window frame is separated from the door guide frame 100 as illustrated in FIG. 37 and then the sliding window 400 is removed (or opened) from the door guide frame 100 , for example, wheels of a large truck may also pass over the door guide frame 100 without interference. Here, when it is difficult to support a passage weight only by the rigidity of the pocket guides 130 of the door guide frame 100 , a separate cover plate 700 covering both the building floor surface 600 and the pocket guides 130 may be installed as illustrated in FIG. 37 .
[0085] As described above, a window provided with a pair glass formed by mounting two glass panels 410 to overlap with each other with a gap therebetween and be spaced apart from each other and adhering the glass panels with a sealing member to form vacuum in the gap has been described in detail with reference to the drawings which illustrate the sliding windows 400 according to the embodiments of the present invention. However, the scope of the present invention to be protected is not limited thereto and may cover various types of sliding windows (door or window) to which the present invention is applied, and various modifications and changes using the basic concept of the present invention defined in the accompanying claims also belong to the scope of the present invention. | The present invention relates to a door guide frame for guiding the sliding movement of a roller device which supports a sliding window and provides a sliding opening/closing operation and, more specifically, to a sliding window installation structure which: stably supports and moves a sliding window on a bottom surface and an upper surface on which the sliding window is installed; reduces an installation space by minimizing the size of a door guide frame and a roller device for supporting a heavy sliding window, thereby obtaining a wider open view when applied to a window; enables vertical stiffeners having an expanded cross section (cross section thicker than glass) for compensating a transverse bending rigidity of glass to be connected to both sides of the glass which constitutes the sliding window formed by including the glass that is supported by a roller; and enables the sliding window with the vertical stiffeners to be installed within the door guide frame in an integrated manner and the sliding window to be detached from the door guide frame in which the sliding window includes the vertical stiffeners. | 4 |
BACKGROUND
[0001] 1. Field of the Disclosure
[0002] Generally, the present disclosure relates to highly sophisticated integrated circuits, including transistors having three-dimensional channel architecture, such as FinFETs, and to a manufacturing method thereof capable of improving the electrical characteristics of the transistor.
[0003] 2. Description of the Related Art
[0004] The fabrication of advanced integrated circuits, such as CPUs, storage devices, application specific integrated circuits (ASICs) and the like, requires the formation of a large number of circuit elements on a given chip area according to a specified circuit layout, wherein field effect transistors represent one important type of circuit element that substantially determines performance of the integrated circuits. Generally, a plurality of process technologies are currently practiced, wherein, for many types of complex circuitry, including field effect transistors, MOS technology is currently one of the most promising approaches due to the superior characteristics in view of operating speed and/or power consumption and/or cost efficiency. During the fabrication of complex integrated circuits using, for instance, MOS technology, millions of transistors, e.g., N-channel transistors and/or P-channel transistors, are formed on a substrate including a crystalline semiconductor layer. A field effect transistor, irrespective of whether an N-channel transistor or a P-channel transistor is considered, typically includes so-called PN junctions that are formed by an interface of highly doped regions, referred to as drain and source regions, with a slightly doped or non-doped region, such as a channel region, disposed adjacent to the highly doped regions. In a field effect transistor, the conductivity of the channel, i.e., the drive current capability of the conductive channel, is controlled by a gate electrode formed adjacent to the channel and separated therefrom by a thin insulating layer. The conductivity of the channel, upon formation of a conductive channel due to the application of an appropriate control voltage to the gate electrode, depends on, among other things, the dopant concentration, the mobility of the charge carriers and, for a planar transistor architecture, the distance between the source and drain, which is also referred to as channel length.
[0005] In view of further device scaling based on well-established materials, new transistor configurations have been proposed in which a “three-dimensional” architecture is provided in an attempt to obtain a desired channel width, while at the same time superior controllability of the current flow through the channel is preserved. To this end, so-called FinFETs have been proposed in which a thin sliver or fin of silicon is formed in a thin active layer of an SOI (silicon-on-insulator) or a standard silicon substrate, wherein, on both sidewalls and, if desired, on a top surface, a gate dielectric material and a gate electrode material are provided, thereby realizing a multiple gate transistor whose channel may be fully depleted.
[0006] In some conventional approaches for forming FinFETs, the fins are formed as elongated device features followed by the deposition of the gate electrode materials, possibly in combination with any spacers, and thereafter the end portions of the fins may be “merged” by epitaxially growing a source or drain material. In particular, several FinFETs can be connected in parallel in this manner, in order to increase the total drive current. Usually then, in order to realize such parallel connection, the individual FinFETs use the same source and/or drain region.
[0007] This, however, has a negative effect on the electrical performances of the FinFET transistors. Among various problems, such an approach with a common source and drain for all FinFETs increases parasitic capacitances between the source and the gate, as well as between the drain and the gate, and it limits the stress type and amount thereof that can be obtained on each of the FinFETs.
[0008] In view of the situation described above, the present disclosure relates to semiconductor devices and manufacturing techniques in which FinFETs, or generally three-dimensional transistors, may be formed and potentially connected in parallel to each other while avoiding or at least reducing the effect of one or more of the problems identified above.
SUMMARY OF THE DISCLOSURE
[0009] The following presents a simplified summary of the disclosure in order to provide a basic understanding of some aspects of the subject matter that is described in further detail below. This summary is not an exhaustive overview of the disclosure, nor is it intended to identify key or critical elements of the subject matter disclosed here. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
[0010] The present disclosure is generally directed to semiconductor devices wherein FinFET devices, or generally three-dimensional transistors, may be formed utilizing a common drain and/or source region for a plurality of devices, and subsequently etching the drain and/or source region so as to remove at least part of the drain and/or source region positioned between the FET fins, or channels. Alternatively, the drain and/or source regions can be formed with such a mask so as to obtain the same geometry, namely, by having less material from the drain and/or source region in between the FET fins than on the fins themselves. This provides the advantage that the surface area of the drain and/or source region facing the gate is reduced, due to the removal, or the absence during the deposition, of the drain and/or source material, thus reducing the amount of parasitic capacitance between the drain region and the gate and/or between the source region and the gate. Further, by limiting the amount of material of the drain and/or source region in between the channels, structural stress caused by the presence of the drain and/or source material can be controlled differently with respect to the case where the drain and/or source material is present between the various fins. Even further, since more space between the fins is left available due to the at least partial absence of the drain and/or source material, it is possible to further deposit a different material, allowing a further degree of control of the stress of the fins.
[0011] In one illustrative embodiment, a semiconductor device is disclosed that includes a plurality of spaced apart fins, wherein each of the plurality of spaced apart fins includes a semiconductor material. Furthermore, the disclosed semiconductor device includes a dielectric material layer that is positioned between each of the plurality of spaced apart fins, and a common gate structure that is positioned above the dielectric material layer and extends across each of the plurality of spaced apart fins. Additionally, the device further includes, among other things, a continuous merged semiconductor material region positioned on each of the plurality of spaced apart fins and above the dielectric material layer, wherein the continuous merged semiconductor material region is laterally spaced apart from the common gate structure and extends between and physically contacts each of the plurality of spaced apart fins. The continuous merged semiconductor material region also has a first sidewall surface that faces toward the common gate structure and a second sidewall surface that is opposite of the first sidewall surface and faces away from the common gate structure. Moreover, a stress-inducing material is positioned in a space that is defined by at least the first sidewall surface of the continuous merged semiconductor material region, opposing sidewall surfaces of an adjacent pair of the plurality of spaced apart fins, and an upper surface of the dielectric material layer.
[0012] Another exemplary embodiment is directed to a semiconductor device that includes, among other things, a plurality of spaced apart fins, each of the plurality of spaced apart fins including a semiconductor material. Additionally, the semiconductor device further includes a dielectric material layer that is positioned between each of the plurality of spaced apart fins, and a common gate structure that is positioned above the dielectric material layer and extends across each of the plurality of spaced apart fins. Furthermore, the illustrative device also includes a continuous merged semiconductor material region that is positioned on each of the plurality of spaced apart fins and above the dielectric material layer, wherein the continuous merged semiconductor material region is laterally spaced apart from the common gate structure and extends between and physically contacts each of the plurality of spaced apart fins. Moreover, the continuous merged semiconductor material region has a first sidewall surface that faces toward the common gate structure and a second sidewall surface that is opposite of the first sidewall surface and faces away from the common gate structure. Additionally, the first sidewall surface of the continuous merged semiconductor material region, a first portion of opposing sidewall surfaces of an adjacent pair of the plurality of spaced apart fins, and a first portion of an upper surface of the dielectric material layer at least partially define a first space between the continuous merged semiconductor material region and the common gate structure, and the second sidewall surface of the continuous merged semiconductor material region, a second portion of the opposing sidewall surfaces of the adjacent pair of the plurality of spaced apart fins, and a second portion of the upper surface of the dielectric material layer at least partially define a second space on an opposite side of the continuous merged semiconductor material region from the first space.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The disclosure may be understood by reference to the following description taken in conjunction with the accompanying drawings, in which like reference numerals identify like elements, and in which:
[0014] FIG. 1 a schematically illustrates a top view of a semiconductor structure according to illustrative embodiments;
[0015] FIG. 1 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 1 a, according to illustrative embodiments;
[0016] FIG. 1 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 1 a , according to illustrative embodiments;
[0017] FIG. 1 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 1 a , according to illustrative embodiments;
[0018] FIG. 2 a schematically illustrates a top view of the semiconductor structure of FIG. 1 a in another manufacturing stage, according to illustrative embodiments;
[0019] FIG. 2 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 2 a , according to illustrative embodiments;
[0020] FIG. 2 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 2 a , according to illustrative embodiments;
[0021] FIG. 2 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 2 a , according to illustrative embodiments;
[0022] FIG. 3 a schematically illustrates a top view of the semiconductor structure of FIG. 1 a in another manufacturing stage, according to illustrative embodiments;
[0023] FIG. 3 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 3 a , according to illustrative embodiments;
[0024] FIG. 3 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 3 a , according to illustrative embodiments;
[0025] FIG. 3 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 3 a , according to illustrative embodiments;
[0026] FIG. 4 a schematically illustrates a top view of the semiconductor structure of FIG. 1 a in another manufacturing stage, according to illustrative embodiments;
[0027] FIG. 4 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 4 a , according to illustrative embodiments;
[0028] FIG. 4 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 4 a , according to illustrative embodiments;
[0029] FIG. 4 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 4 a , according to illustrative embodiments;
[0030] FIG. 5 a schematically illustrates a top view of the semiconductor structure of FIG. 1 a in another manufacturing stage, according to illustrative embodiments;
[0031] FIG. 5 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 5 a , according to illustrative embodiments;
[0032] FIG. 5 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 5 a , according to illustrative embodiments;
[0033] FIG. 5 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 5 a , according to illustrative embodiments;
[0034] FIG. 6 a schematically illustrates a top view of the semiconductor structure of FIG. 1 a in another manufacturing stage, according to illustrative embodiments;
[0035] FIG. 6 b schematically illustrates a cross-sectional view along section A-A′ of FIG. 6 a , according to illustrative embodiments;
[0036] FIG. 6 c schematically illustrates a cross-sectional view along a section B-B′ of FIG. 6 a , according to illustrative embodiments;
[0037] FIG. 6 d schematically illustrates a cross-sectional view along a section C-C′ of FIG. 6 a , according to illustrative embodiments;
[0038] FIG. 7 a schematically illustrates a top view of a semiconductor structure, according to illustrative embodiments; and
[0039] FIG. 7 b schematically illustrates a top view of a semiconductor structure, according to illustrative embodiments.
[0040] While the subject matter disclosed herein is susceptible to various modifications and alternative forms, specific embodiments thereof have been shown by way of example in the drawings and are herein described in detail. It should be understood, however, that the description herein of specific embodiments is not intended to limit the invention to the particular forms disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
DETAILED DESCRIPTION
[0041] Various illustrative embodiments of the present subject matter are described below. In the interest of clarity, not all features of an actual implementation are described in this specification. It will of course be appreciated that in the development of any such actual embodiment, numerous implementation-specific decisions must be made to achieve the developers' specific goals, such as compliance with system-related and business-related constraints, which will vary from one implementation to another. Moreover, it will be appreciated that such a development effort might be complex and time-consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art having the benefit of this disclosure.
[0042] The present subject matter will now be described with reference to the attached figures. Various systems, structures and devices are schematically depicted in the drawings for purposes of explanation only and so as to not obscure the present disclosure with details that are well known to those skilled in the art. Nevertheless, the attached drawings are included to describe and explain illustrative examples of the present disclosure. The words and phrases used herein should be understood and interpreted to have a meaning consistent with the understanding of those words and phrases by those skilled in the relevant art. No special definition of a term or phrase, i.e., a definition that is different from the ordinary and customary meaning as understood by those skilled in the art, is intended to be implied by consistent usage of the term or phrase herein. To the extent that a term or phrase is intended to have a special meaning, i.e., a meaning other than that understood by skilled artisans, such a special definition will be expressly set forth in the specification in a definitional manner that directly and unequivocally provides the special definition for the term or phrase.
[0043] The following embodiments are described in sufficient detail to enable those skilled in the art to make use of the invention. It is to be understood that other embodiments would be evident, based on the present disclosure, and that system, structure, process or mechanical changes may be made without departing from the scope of the present disclosure. In the following description, numeral-specific details are given to provide a thorough understanding of the disclosure. However, it will be apparent that the embodiments of the disclosure may be practiced without the specific details. In order to avoid obscuring the present disclosure, some well-known circuits, system configurations, structure configurations and process steps are not disclosed in detail.
[0044] Generally, the present disclosure contemplates manufacturing techniques and semiconductor devices in which a non-planar transistor configuration, also referred to as a three-dimensional transistor or, more specifically, a FinFET, may be provided on the basis of a process strategy in which initial fins formed from semiconductor-based materials, such as silicon, may be used.
[0045] FIG. 1 a schematically illustrates a top view of a semiconductor structure 100 . FIGS. 1 b, 1 c and 1 d schematically illustrate cross-sectional views of the semiconductor structure 100 taken along lines A-A′, B-B′ and C-C′, respectively.
[0046] As can be seen in the figures, the semiconductor structure 100 includes a substrate 101 in which fins 102 a - 102 c are provided. At least part of the fins 102 a - 102 c acts as a channel for the respective FinFET, as will be described in more detail later. The fins 102 a - 102 c may be realized by etching material from the substrate 101 , so as to expose the fins 102 a - 102 c , or by a deposition of material onto the substrate 101 so as to build the fins 102 a - 102 c . Still alternatively, they could be realized by a sidewall image transfer method. In all cases, the resulting structure is the one illustrated in FIGS. 1 a - 1 d. The material of the substrate 101 may silicon or any other suitable semiconductor material based on the specific device requiremenst, such as germanium (Ge), silicon/germanium (SiGe) or a layered semiconductor structure, such as a silicon-on-insulator (SOI), or a semiconductor alloy, such as a III-V alloy. The fins 102 a - 102 c may be realized from the same semiconductor material of the substrate 101 , in particular when obtained by removing material from the substrate 101 , but also when realized by deposition of material on the substrate 101 , for instance, when using a silicon epitaxial growth on a silicon substrate. Alternatively, the fins 102 a - 102 c may be realized by a different semiconductor material. In both cases, the fins 102 a - 102 c may be doped differently with respect to the substrate 101 .
[0047] As can be seen in FIG. 1 b , the fins 102 a - 102 c extend in a vertical Y direction, preferably with a height T 1 included in the range of 60-90 nm, even more preferably with a value of 70 nm. Furthermore, each of the fins 102 a - 102 c has a width W 1 in the X direction, preferably in the range of 20-40 nm, even more preferably with a value of 25 nm. Finally, as can be seen in FIG. 1 c , the fin 102 b , as well as fins 102 a and 102 c (not illustrated in FIG. 1 c ), have a length L 1 in the Z direction, preferably in the range of 50-80 nm, even more preferably with a value of 60 nm. Also, the fins 102 a - 102 c may be placed at a distance W 2 from each other, in the X direction, in the range from 20-40 nm, preferably 35 nm.
[0048] Each of the fins 102 a - 102 c may sustain a maximum flow of current, which is limited by the materials and the dimensions used. For some applications, a level of current higher than the one sustainable by a single FinFET may be needed. In those cases, the fins 102 a - 102 c may be connected in parallel by realizing a common source region and/or a common drain region for at least two of the fins 102 a - 102 c , in order to increase the total current flowing between the common source region and/or the common drain region. The realization of such common drain and/or source region will be described in the following description, in particular with reference to FIGS. 4 a - 4 d.
[0049] FIGS. 2 a -2 d schematically illustrate a semiconductor structure 200 , resulting from the semiconductor structure 100 following a further manufacturing step. In particular, FIGS. 2 a -2 d schematically illustrate the semiconductor structure from the same viewpoints of FIGS. 1 a - 1 d, respectively.
[0050] As can be seen in FIGS. 2 a -2 d , the semiconductor structure 200 is obtained from the semiconductor structure 100 by a deposition of an insulating layer 103 . Preferably, in some embodiments, the insulating layer 103 may be deposited with a thickness in the Y direction of 100 nm. Subsequently, the insulating layer 103 may be thinned down with a chemical mechanical polishing (CMP) step, to roughly the height value corresponding to the top surface of the fins 102 a - 102 c . Finally, the insulating layer 103 may be anisotropically etched so as to leave a layer of insulating material with a thickness T 2 of, preferably, 50 nm, at the bottom of the fins 102 a - 102 c . In other words, in some embodiments, the insulating layer 103 has a height which is smaller than the height of the fins 102 a - 102 c.
[0051] Although the above process steps have been provided so as to illustrate one exemplary embodiment for realizing the insulating layer 103 , it will be clear to those skilled in the art that the insulating layer 103 may be realized within the fins 102 a - 102 c with alternative process steps. For instance, the insulating layer 103 could be deposited only within the space between the fins 102 a - 102 c , by use of the appropriate mask and deposition steps, so as to achieve the required thickness in a single deposition step, without the use of any CMP and/or etching.
[0052] FIGS. 3 a -3 d schematically illustrate a semiconductor structure 300 , resulting from the semiconductor structure 200 following a further manufacturing step. In particular, FIGS. 3 a -3 d schematically illustrate the semiconductor structure from the same viewpoints of FIGS. 1 a -1 d , respectively.
[0053] As can be seen in FIG. 3 a , a dummy gate 104 is realized on the semiconductor structure 200 , thereby resulting in the semiconductor structure 300 . Although a dummy gate is here described, thereby signifying that in subsequent processes, not illustrated, a gate will replace the dummy gate, the present invention is not limited thereto. In particular, in some embodiments, the gate 104 may be the final gate and not a dummy gate. Thus, in describing the present invention, the term “dummy gate 104 ” and “gate 104 ” may be used interchangeably.
[0054] In particular, the dummy gate 104 may be realized, for instance, by polysilicon. Preferably, the dummy gate 104 has a width along direction Z, corresponding to the channel length of the FinFETs in the range of 20-30 nm, even more preferably with the value of 26 nm. In other words, the part of the fins 102 a - 102 c under the dummy gate 104 corresponds to the channel of the respective FinFET. The dummy gate 104 is separated by each of the fins 102 a - 102 c by a gate dielectric 105 , as can be seen in FIGS. 3 b - 3 d. The gate dielectric 105 is typically an oxide, such as a silicon oxide, preferably having a thickness of 2-3 nm. The gate dielectric 105 may be obtained, for instance, by a chemical vapor deposition or by any other technique allowing the realization of a thin layer on the fins 102 a - 102 c . The dummy gate 104 may be obtained by a deposition of the material realizing the dummy gate 104 , followed by a subsequent planarization via a CMP step.
[0055] Although not illustrated in the figures, a nitride layer may be realized on top of the dummy gate 104 , and/or parts of the fins where the source and drain do not need to be realized, and/or of the insulating layer. The purpose of such a nitride layer is to act as a spacer during the subsequent growth of the source and drain regions 108 and 109 ( FIGS. 4 a -4 d ). In this respect, it will be clear to those skilled in the art that such a spacing layer is not necessarily made of nitride, but that any material allowing the subsequent realization of the source and drain in a localized manner may be employed.
[0056] FIGS. 4 a -4 d schematically illustrate a semiconductor structure 400 , resulting from the semiconductor structure 300 following a further manufacturing step. In particular, FIGS. 4 a -4 d schematically illustrate the semiconductor structure from the same viewpoints of FIGS. 1 a -1 d , respectively.
[0057] More specifically, in the semiconductor structure 400 , the source and drain regions 108 and 109 are realized on the two ends of each of the fins 102 a - 102 c . By using the previously mentioned nitride layer, or any equivalent masking layer, the positioning of the source and drain regions 108 and 109 may be precisely controlled. In particular, the shape of the source and drain regions 108 and 109 corresponds to the negative image of the nitride, or masking, layer mentioned with reference to FIGS. 3 a -3 d and not illustrated.
[0058] The realization of the source region 108 and the drain region 109 may be done, in some embodiments, by using an epitaxial growth of silicon to merge the fins at their end in the regions 108 and 109 , namely, in those regions not covered by the masking or nitride (SiN) layer. Thanks to the nitride or masking layer, the proximity of the source and drain regions 108 and 109 to the dummy gate 104 may be precisely controlled. In an exemplary manufacturing method, the gate 104 is completely encapsulated with nitride and only the future region of the source and drain 108 and 109 are open by a lithography step followed by a corresponding etching step so that selective silicon is grown in those regions. Although the source and drain regions 108 and 109 are here described as being the result of a silicon epitaxial growth, the present invention is not limited thereto and other materials, such as SiGe or III-V alloys, and/or other deposition methods, such as a chemical vapor deposition (CVD) or physical vapor deposition (PVD), may be employed instead. The source and drain regions 108 and 109 may then be subsequently doped, if necessary, for instance by using boron for P-type FETs and P/As for N-type FETs. The source and drain regions 108 and 109 may be placed at a distance W 3 , in the Z direction, in the range of 10-30 nm, preferably 20 nm, from the gate 104 . Additionally, they may have a width W 4 , in the Z direction, in the range of 20-40 nm, preferably 30 nm.
[0059] Following the realization of the source and drain regions 108 and 109 , the fins 102 a - 102 c are thus electrically connected in parallel. To access the source and drain regions 108 and 109 , corresponding source and drain contacts (not illustrated) may be realized on the source and drain regions. However, such a construction provides a rather wide area of the source and drain regions 108 and 109 , on the XY plane, facing the gate 104 . This creates a rather high parasitic capacitance between the source region 108 and the gate 104 , as well as between the drain region 109 and the gate 104 . Additionally, the material of the source and drain regions 108 and 109 may present a bi-axial stress, due to the growing technique employed for those regions. This may limit the amount of current that can flow through the fins 102 a - 102 c , and/or through the source and drain regions 108 and 109 .
[0060] FIGS. 5 a -5 d schematically illustrate a semiconductor structure 500 , corresponding to the semiconductor structure 400 with an overlapping mask 107 . In particular, FIGS. 5 a -5 d schematically illustrate the semiconductor structure from the same viewpoints of FIGS. 1 a - 1 d, respectively.
[0061] More specifically, in FIG. 5 a , a mask 107 is illustrated as vertically overlapping the semiconductor structure 500 . Here, for a reduction in the number of masks and thereby in the manufacturing costs, the mask 107 may correspond to the mask (not illustrated) already used for the realization of the fins 102 a - 102 c . Here, even if the mask 107 is positioned with a tolerance of 5-10 nm with respect to its original placement for realizing the fins 102 a - 102 c , the removing step may still be carried out successfully. However, any mask that allows the removal of at least part of the material of the source and drain regions 108 and 109 in at least part of the region R 1 separating the fins 102 a - 102 c from each other may be used instead. Thanks to the use of the mask 107 , selective removal of the material used for the source and drain regions 108 and 109 in the regions R 1 between the fins 102 a - 102 c is achieved. The area between the gate 104 and the source and drain regions 108 and 109 may, at this stage, be still protected by the silicon nitride or, more generally, the masking layer from the spacer, used in the previous manufacturing step, so that material of the source and drain regions 108 and 109 may be selectively removed in the portion between the fins 102 a - 102 c , without affecting the rest of the structure.
[0062] FIGS. 6 a -6 d schematically illustrate a semiconductor structure 600 , corresponding to the semiconductor structure 400 after the etching process based on the mask 107 has been carried out. In particular, FIGS. 6 a -6 d schematically illustrate the semiconductor structure from the same viewpoints of FIGS. 1 a -1 d , respectively.
[0063] Thanks to the removal of the material of the source and drain regions 108 and 109 in regions R 1 between the fins 102 a - 102 c , the semiconductor structure 600 as illustrated in FIGS. 6 a -6 d may be obtained. In particular, as can be seen in FIG. 6 a , the regions R 1 placed between the fins 102 a - 102 c , aligned with the source and drain regions 108 and 109 in the X direction, do not contain material connecting the sources and drains 108 and 109 to each other. Rather, the source and drain regions 108 and 109 are each independently separated for each fin 102 a - 102 c , thus resulting in independent sources 108 a - 108 c and independent drains 109 a - 109 c.
[0064] It should be noted that, in the present embodiment, the mask 107 has been illustrated as covering the entire illustrated source and drain regions 108 and 109 in the Z direction. However, the present invention is not limited thereto. In particular, the source and drain material between the fins 102 a - 102 c may be completely removed, as illustrated in FIGS. 6 a -6 d so as to leave each fin with an independent source 108 a - 108 c and drain 109 a - 109 c . Those independent sources and drains may then be electrically connected via their respective contacts and the appropriate use of vias and connection lines.
[0065] Alternatively, only a portion of the source and drain material may be removed from between the fins 102 a - 102 c , in particular the portion closest, in the Z direction, to the dummy gate 104 , as illustrated in FIG. 7 b by the semiconductor structure 800 . Here, material of the drain and source regions 108 and 109 may be left between the fins 102 a - 102 c at a position further away, in the Z direction, from the dummy gate 104 than the source and drain 108 g - 108 i and 109 g - 109 i on the fins 102 a - 102 c . In particular, the remaining material of the source and drain regions 108 and 109 may start at a distance W 5 , in the Z direction, in the range of 20-30 nm, preferably 25 nm. Thanks to the latter approach, connection between the sources and drains 108 g - 108 i and 109 g - 109 i of the fins 102 a - 102 c may be ensured by means of the remaining material of the source and drain regions 108 and 109 in between the fins 102 a - 102 c.
[0066] Still alternatively. only a portion of the source and drain material may be removed from between the fins 102 a - 102 c , in particular the portion further away, in the Z direction, from the dummy gate 104 , as illustrated in FIG. 7 a by the semiconductor structure 700 . Here, material of the drain and source regions 108 and 109 may be left between the fins 102 a - 102 c at a position as close as, in the Z direction, the dummy gate 104 than the sources and drains 108 d - 108 f and 109 d - 109 f on the fins 102 a - 102 c . Thanks to this approach, connection between the sources and drains 108 d - 108 f and 109 d - 109 f of the fins 102 a - 102 c may be ensured by means of the remaining material of the source and drain regions 108 and 109 in between the fins 102 a - 102 c.
[0067] The embodiments illustrated by semiconductor structures 700 and 800 , could, for instance, be employed in order to increase the mechanical strength of the fins 102 a - 102 c.
[0068] Both in the semiconductor structure 700 and 800 , the width, in the Z direction, of the remaining source and drain material may have a width W 6 , in the Z direction, in the range of 10-20 nm, preferably 15 nm.
[0069] Thus, thanks to the described process, a semiconductor structure may include at least a first and a second three-dimensional transistor, the first transistor and the second transistor being electrically connected in parallel to each other and sharing a common gate 104 , may be obtained, in which each transistor has a source region and a drain region, wherein the source and/or drain regions of the first transistor may be at least partially separated from, respectively, the source 108 a - 108 i and/or drain 109 a - 109 i of the second transistor. Even more specifically, each of the first and second transistors may include a channel, and the source and/or drain of the first transistor are at least partially separated from, respectively, the source and/or drain of the second transistor along a direction parallel to the channel of the first transistor and/or the channel of the second transistor. Further, the sources 108 a - 108 c , 108 g - 108 i and/or drains 109 a - 109 c , 109 g - 109 i of the first transistor are at least partially separated from, respectively, the sources 108 a - 108 c , 108 g - 108 i and/or drains 109 a - 109 c , 109 g - 109 i of the second transistor in the part of the source and/or drain closest to gate 104 . Alternatively, the sources 108 d - 108 f and/or drains 109 a - 109 f of the first transistor are at least partially separated from, respectively, the sources 108 d - 108 f and/or drains 109 a - 109 f of the second transistor in the part of the source and/or drain furthest from the gate 104 . Still alternatively, the sources 108 a - 108 c and/or drains 109 a - 109 c of the first transistor are completely separated from, respectively, the sources 108 a - 108 c and/or drains 109 a - 109 c of the second transistor. In such embodiments, each transistor further includes a channel, and the source and/or drain of the first transistor have a width W 1 corresponding to a channel's width of the first transistor, and/or the source and/or drain of the second transistor have a width W 1 corresponding to a channel's width of the second transistor. Here, the expression partially separated is intended to mean that the two elements are not completely connected along their sides facing each other, but only a part of the side facing each other is employed for the connection to the other element.
[0070] More generally, the present invention may be implemented by either completely removing the material in regions R 1 , as illustrated in the semiconductor structure 600 , or by removing only part of it, as illustrated in the semiconductor structures 700 and 800 . It will be clear to those skilled in the art that the semiconductor structures 700 and 800 are only two extreme situations of the same configuration in which some material of the source and drain regions 108 and 109 is left in the regions R 1 , and that configurations in between those two may be implemented.
[0071] Thus, semiconductor structures 600 - 800 differ from semiconductor structure 400 due to the removal of at least part of the drain and source material between the fins 102 a - 102 c , namely in the regions R 1 . In particular, in the semiconductor structures 600 and 800 , due to the removal of such material in the proximity of the dummy gate 104 , it is possible to reduce the capacitance between the dummy gate 104 and the source and drain regions 108 and 109 . In fact, as can be seen when comparing the semiconductor structure 600 and 800 with the semiconductor structure 400 , the area on the XY plane of the sources and drains 108 a - 108 c and 109 a - 109 c of the semiconductor structure 600 is substantially smaller than the equivalent area for the semiconductor structure 400 . Even in the case of the semiconductor structure 800 , where only some of the material forming the source and drain regions 108 and 109 is removed from between the fins 102 a - 102 c , while the area on the XY plane of the source and drain regions 108 and 109 of the semiconductor structure 800 and 400 is the same, the average distance of such area from the gate 104 is higher for the semiconductor structure 800 than for the semiconductor structure 400 . That is, both when only some of the material of the source and drain regions 108 and 109 is removed, or when all of such material is removed, the capacitance between the source and drain regions 108 and 109 and the dummy gate 104 is reduced, thus improving the electrical characteristics of the FinFETs connected in parallel.
[0072] Additionally, by removing material in between the fins 102 a - 102 c , it is possible to convert a biaxial stress from the epitaxial growth of the drain and source 108 and 109 material, such as, for instance, silicon/germanium, into uniaxial stress. In some conditions, in fact, the uniaxial stress in FinFETs achieves a better mobility improvement compared to the biaxial stress. Thus, the semiconductor structures 600 , 700 and 800 have better electrical characteristics than the semiconductor structure 400 , in which the material between the fins 102 a - 102 c creates a biaxial stress on the fins, not present or reduced in the semiconductor structures 600 , 700 and 800 .
[0073] Still further, the space between the independent sources and drains 108 a - 108 c and 109 a - 109 c of neighboring fins 102 a - 102 c in the semiconductor structure 600 , created by the complete removal of the source and drain material, as well as the space between sources and drains 108 d - 108 i and 109 d - 109 i of neighboring fins 102 a - 102 c in the semiconductor structures 700 and 800 , created by the partial removal of the source and drain material, may be subsequently filled with a different material, such as a stress overlayer film, for instance, silicon-nitride (Si 3 N 4 ), silicon-oxide (SiO 2 ), etc., thus enabling a mobility and drive current improvement. That is, thanks to the use of another material, it is possible to further configure the desired stress on the fins 102 a - 102 c and/or on the sources and drains 108 a - 108 i and 109 a - 109 i so as to improve the respective electrical characteristics of the FinFETs based on the fins 102 a - 102 c . Such a further configuration of the stress of the source and drain is not possible in the semiconductor structure 400 , where the space R 1 between the source and drain regions 108 and 109 of the fins 102 a - 102 c is completely filled by the same source and drain region material.
[0074] Although not illustrated, it will be clear to those skilled in the art that some process steps not shown in the figures, such as an RTA for activation and diffusion, and/or a silicide formation, and/or a dummy gate removal and replacement by a high-k/metal gate step, and/or contact formation and BEOL processing as in a conventional FinFET flow have not been illustrated for the sake of clarity.
[0075] In alternative embodiments of the present invention, instead of removing the material of the source and drain regions 108 and 109 in between the fins 102 a - 102 c , it is possible to deposit such material only in correspondence with zones illustrated by reference numerals 108 a - 108 i and 109 a - 109 i in the semiconductor structures 600 - 800 . In other words, instead of realizing a deposition of source and drain regions 108 and 109 and a subsequent patterning thereof by means of, for instance, photolithography and etching, it is possible to proceed directly to the localized deposition of sources and drains 108 a - 108 i and 109 a - 109 i in a localized manner. This could be achieved, for instance, by using the mask 700 for the localized deposit of the material of the source and drain regions 108 and 109 , in addition to the above-mentioned nitride layer, or more generally a masking layer, covering the dummy gate 104 and acting as a spacer in the Z direction for defining the distance between the source 108 and the dummy gate 104 , as well as the distance between the drain 109 and the dummy gate 104 . Still in other terms, such localized realization of the sources and drains 108 a - 108 c and 109 a - 109 c could be achieved by using the mask 107 for the deposition step illustrated in FIGS. 4 a - 4 d.
[0076] Moreover, although three fins 102 a - 102 c have been illustrated, it will be clear to those skilled in the art that any number of fins higher than two may be used to implement the present invention.
[0077] The particular embodiments disclosed above are illustrative only, as the invention may be modified and practiced in different but equivalent manners apparent to those skilled in the art having the benefit of the teachings herein. For example, the method steps set forth above may be performed in a different order. Furthermore, no limitations are intended by the details of construction or design herein shown, other than as described in the claims below. It is therefore evident that the particular embodiments disclosed above may be altered or modified and all such variations are considered within the scope and spirit of the invention. Accordingly, the protection sought herein is as set forth in the claims below. | A semiconductor device includes a plurality of spaced apart fins, a dielectric material layer positioned between each of the plurality of spaced apart fins, and a common gate structure positioned above the dielectric material layer and extending across the fins. A continuous merged semiconductor material region is positioned on each of the fins and above the dielectric material layer, is laterally spaced apart from the common gate structure, extends between and physically contacts the fins, has a first sidewall surface that faces toward the common gate structure, and has a second sidewall surface that is opposite of the first sidewall surface and faces away from the common gate structure. A stress-inducing material is positioned in a space defined by at least the first sidewall surface, opposing sidewall surfaces of an adjacent pair of fins, and an upper surface of the dielectric material layer. | 7 |
FIELD OF THE INVENTION
The present invention relates to a catalyst for synthesizing 1-hexene from ethylene trimerization and application thereof.
BACKGROUND OF THE INVENTION
EP 699648 discloses a Cr-based catalyst, which comprises a chromic salt A, an organic aluminide B, a pyrrole compound C and a 13(IIIB) chloride or 14(VIB) chloride. The best chromic salts include chromium 2-ethylhexanoate, chromium naphthenate and chromium acetylacetone. A, B and D have effect on the catalytic activity, and C influences the selectivity of 1-hexene. The selectivity of 1-hexene is 80%, and the purity is 98-99%. The advantages are that 1-hexene is used as solvent for catalyst preparation and ethylene trimerization, thus the apparatus for separation of solvent with 1-hexene and cost thereof are omitted.
EP 0608447A discloses a Cr-based catalyst composition as the catalyst for ethylene oligomerization and/or copolymerization, in which the catalyst composition contains a Cr-containing compound, a pyrrole compound, a Lewis acid and/or metal alkyl compound as an activator, and optionally a halogen source which can be either inorganic halides or various organic halides. The catalyst has high 1-hexene selectivity, but with low catalytic activity.
JP 0832519 discloses Sn(OSO 2 F 3 ) 2 compound is used in place of halogen source as mentioned above in EP 0608447A, thus to form a new quaternary Cr-based catalyst composition. The activity and selectivity of this composition have not been improved significantly.
U.S. Pat. No. 5,910,619 discloses 1,2,3,4,5,6-hexachlorocyclohexane is used as improver to form a quaternary catalyst composition, the catalytic activity of which is improved slightly. CN 1294109A (the title of which is a catalyst for preparing 1-hexene from ethylene oligomerization and application thereof) discloses a new catalyst system, the catalytic activity of which is improved greatly. However, these catalysts cannot meet current requirements yet. There is still a need for improving the property of catalyst so as to increase catalytic activity.
In the ethylene oligomerization as disclosed in WO2004/05647, the content of 1-octylene is at most 69.3%, and the content of 1-hexene is 10-20%.
SUMMARY OF THE INVENTION
The aim of the present application is to develop a catalyst containing (a) the compound containing P and N, (b) electron donor, (c) Cr compound, (d) carrier and (e) accelerator. This catalyst is used for preparing 1-hexene from ethylene trimerization. Cr compound can form three unoccupied orbitals under the effect of ligand and accelerator, which may facilitate the coordination of ethylene molecular, and then β-H elimination reaction occurs to obtain 1-hexene. And the by-product polyethylene is more easily formed on the carrier SiO 2 so as to avoid sticking to the apparatus and facilitate long periodic run of reactor.
The present application is directed to a Cr catalyst system used for ethylene trimerization, which is the composition containing the following:
(1) compound (a) containing P and N, with formula:
wherein R 1 , R 2 , R 3 and R 4 independently are selected from the group consisting of phenyl, benzyl and naphthyl, R 5 is selected from the group consisting of isopropyl, butyl, cyclopropyl, cyclopentyl, cyclohexyl and fluorenyl;
(2) electron donor (b), which is 1,4-dichlorobenzene, 1,1,2-trichloroethane, 1,2-dichlorethane, chlorobenzene, 1,2-dichlorobenzene, 1,3-dichlorobenzene and/or 1,4-dichlorobenzene;
(3) Cr compound (c), which is chromium isooctoate, chromium chloride tetrahydrofuran and/or chromium acetylacetonate;
(4) carrier (d), which is SiO 2 ; and
(5) accelerator (e), which is trimethyl aluminium, triethyl aluminium, tripropyl aluminium, tributyl aluminium and/or triisobutyl aluminium.
The molar ratio of (a), (b), (c), (d) and (e) is 0.5-100:0.5-100:1:0.5-10:50-5000, preferably 1-80:1-70:1:1-8:100-4000.
The five components (a)-(e) can be mixed under inert atmosphere for 10 minutes, then added to reactor, with ethylene introduced to undergo trimerization. Alternatively, the five components (a)-(e) can be directly added to reactor, with ethylene introduced to undergo trimerization. The reaction is usually at the temperature of 30-150° C., preferably of 20-90° C., under the pressure of 0.5-10.0 MPa, preferably of 1-10 MPa, more preferably of 2-6 MPa for 0.1-4 hours, preferably 0.3-1 hours, more preferably 0.5-0.7 hours.
The ethylene trimerization is mainly carried out in an inert solvent. The optional solvents include alkane, aromatic hydrocarbon, halohydrocarbon and alkene and so on. The typical solvents include, but not limited to, benzene, toluene, xylene, isopropylbenzene, n-heptane, n-hexane, methyl cyclohexane, cyclohexane, 1-hexene, 1-octylene and ionic liquids.
The catalyst has high catalytic activity and high 1-hexene selectivity. What is more, by-product polyethylene does not stick to the apparatus.
DETAILED DESCRIPTION OF THE INVENTION
The following examples are only intended to illustrate the present application without limiting the scope of the present application.
Example 1
1. Preparation of (diphenyl)phosphonitryl(cyclopropyl)phosphine(diphenyl) ligand
(1) Preparation of N,N-diisopropyldichlorophosphoamide
To a 250 ml reactor with N 2 sufficient exchange, the dehydrated toluene (100 ml), and PCl 3 (21.87 ml, 0.25 mol) are added under stirring. Then the temperature is reduced to −20° C. At room temperature, diisopropylamine (70 ml, 0.5 mol) is added slowly under stirring. After stirring for 3 hours, the temperature is raised to room temperature and then the reaction is continued for 2 hours. 38.1 g (0.19 mol, 74%) product is finally obtained after filtrating and drying.
(2) Preparation of Grignard Reagent Phenylmagnesium Bromide
To a 250 ml reactor with N 2 sufficient exchange, the dehydrated THF (100 ml), and magnesium powder (9.11 g, 0.375 mol) are added under stirring. The temperature is reduced by ice bath and brombenzene (11.775 g, 0.075 mol) is added dropwise slowly. Two hours later, under heating and refluxing, the reaction is continued for 2 hours. Then Grignard reagent is obtained.
(3) Preparation of Diphenyl Phosphorus Chloride
To a 250 ml reactor with N 2 sufficient exchange, the dehydrated THF (100 ml) is added under stirring. The temperature is reduced to 0° C. N,N-diisopropyldichlorophosphoamide (6.64 ml, 36 mmol) is added slowly. The temperature is raised to room temperature for 12 hours. Then the reaction mixture is diluted with cyclohexane and bubbled with dry H333331 gas for 1 hour. The diphenyl phosphorus chloride is finally obtained after filtrating and drying.
(4) Preparation of (diphenyl)phosphonitryl(cyclopropyl)phosphine(diphenyl)
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated dichlormethane (20 ml), triethylamine (3.75 ml) and diphenyl phosphorus chloride (1.326 ml, 7.2 mmol) are added under stirring. The temperature is reduced to 0° C. The cyclopropylamine (3.6 mmol) is added slowly. The reaction is carried out under stirring for 30 minutes and then raised to room temperature to continue for 12 hours. The product (0.87 g, 56.6%) is finally obtained after filtrating and drying.
2. Preparation of Catalyst
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated toluene (10 ml), (diphenyl)phosphonitryl(cyclopropyl)phosphine(diphenyl) (29 mg), triethylaluminium (10 ml), chromium isooctoate (0.03 mmol), 1,1,2,2-tetrachloroethane (7 ml, 0.54 mmol) and SiO 2 (0.03 mmol) are added. The reaction is undergone at room temperature for 10 minutes to obtain the catalyst for use.
3. Ethylene Trimerization
500 ml autoclave is heated and vacuumed for 2 hours. After N 2 exchange for several times, ethylene is introduced therein. The temperature is reduced to predetermined temperature. The dehydrated toluene (200 ml) and the catalyst as obtained above are added. Oligomerization is carried out at 90° C. under the pressure of 4.0 MPa. After 40 minutes, the temperature is reduced by ice bath, the pressure is relieved, and the reaction is terminated by 10 wt % acidified alcohol. The results are listed in appended Table 1.
Example 2
1. Preparation of (diphenyl)phosphonitryl(cyclopentyl)phosphine(diphenyl) ligand
(1) Preparation of N,N-diisopropyldichlorophosphoamide
The process is the same as that in Example 1.
(2) Preparation of Grignard Reagent Phenylmagnesium Bromide
The process is the same as that in Example 1.
(3) Preparation of Diphenyl Phosphorus Chloride
The process is the same as that in Example 1.
(4) Preparation of (diphenyl)phosphonitryl(cyclopentyl)phosphine(diphenyl)
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated dichlormethane (20 ml), triethylamine (3.75 ml) and diphenyl phosphorus chloride (1.326 ml, 7.2 mmol) are added under stirring. The temperature is reduced to 0° C. The cyclopentylamine (0.415 ml, 3.5 mmol) is added slowly. The reaction is carried out under stirring for 30 minutes and then raised to room temperature to continue for 12 hours. The product (0.55 g, 32.68%) is finally obtained after filtrating and drying.
2. Preparation of Catalyst
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated cyclohexane (10 ml), trimethylaluminium (10 ml), (diphenyl)phosphonitryl(cyclopentyl)phosphine(diphenyl) (31 mg), CrCl 3 .(THF) 3 (12 mg), SiO 2 (0.3 mmol) and 1,1,2,2-tetrabromoethane (0.02, 0.069 mmol) are added. The reaction is undergone at room temperature for 5 minutes to obtain the catalyst for use.
3. Ethylene Trimerization
500 ml autoclave is heated and vacuumed for 2 hours. After N 2 exchange for several times, ethylene is introduced therein. The temperature is reduced to predetermined temperature. The dehydrated cyclohexane (200 ml) and the catalyst as obtained above are added. Oligomerization is carried out at 20° C. under the pressure of 7.0 MPa. After 20 minutes, the temperature is reduced by ice bath, the pressure is relieved, and the reaction is terminated by 10 wt % acidified alcohol. The results are listed in appended Table 1.
Example 3
1. Preparation of (diphenyl)phosphonitryl(fluorenyl)phosphine(diphenyl) ligand
(1) Preparation of N,N-diisopropyldichlorophosphoamide
The process is the same as that in Example 1.
(2) Preparation of Grignard Reagent Phenylmagnesium Bromide
The process is the same as that in Example 1.
(3) Preparation of Diphenyl Phosphorus Chloride
The process is the same as that in Example 1.
(4) Preparation of (diphenyl)phosphonitryl(fluorenyl)phosphine(diphenyl)
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated dichlormethane (20 ml), triethylamine (3.75 ml) and diphenyl phosphorus chloride (1.326 ml, 7.2 mmol) are added under stirring. The temperature is reduced to 0° C. The fluorenamine (0.652 g, 3.6 mmol) is added slowly. The reaction is carried out under stirring for 30 minutes and then raised to room temperature to continue for 12 hours. The product (0.48 g, 24.3%) is finally obtained after filtrating and drying.
2. Preparation of Catalyst
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated cyclohexane (10 ml), tripropylaluminium (10 ml), SiO 2 (0.1 mmol), (diphenyl)phosphonitryl(fluorenyl)phosphine(diphenyl) (35 mg), Cr(acac) 3 (12 mg) and 1,2-dimethoxyethane (0.4 ml, 0.031 mmol) are added. The reaction is undergone at room temperature for 5 minutes to obtain the catalyst for use.
3. Ethylene Trimerization
500 ml autoclave is heated and vacuumed for 2 hours. After N 2 exchange for several times, ethylene is introduced therein. The temperature is reduced to predetermined temperature. The dehydrated benzene (200 ml) and the catalyst as obtained above are added. Oligomerization is carried out at 30° C. under the pressure of 3.0 MPa. After 20 minutes, the temperature is reduced by ice bath, the pressure is relieved, and the reaction is terminated by 10 wt % acidified alcohol. The results are listed in appended Table 1.
Example 4
1. Preparation of 1,4-bis(N(P(phenyl) 2 ) 2 )-benzene ligand
(1) Preparation of N,N-diisopropyldichlorophosphoamide
The process is the same as that in Example 1.
(2) Preparation of Grignard Reagent Phenylmagnesium Bromide
The process is the same as that in Example 1.
(3) Preparation of Diphenyl Phosphorus Chloride
The process is the same as that in Example 1.
(4) Preparation of 1,4-bis(N(P(phenyl) 2 ) 2 )-benzene
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated dichlormethane (20 ml), triethylamine (3.75 ml) and diphenyl phosphorus chloride (1.326 ml, 7.2 mmol) are added under stirring. The temperature is reduced to 0° C. The 1,4-phenylenediamine (0.19 g, 1.8 mmol) is added slowly. The reaction is carried out under stirring for 30 minutes and then raised to room temperature to continue for 12 hours. The product (0.8 g, 52.3%) is finally obtained after filtrating and drying.
2. Preparation of Catalyst
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated cyclohexane (10 ml), tributylaluminium solution (7 ml), SiO 2 (0.3 mmol), 1,4-bis(N(P(phenyl) 2 ) 2 )-benzene (27 mg), chromium 2-ethylhexanoate (10 mg) and 1,2-dichlorethane (0.13 mmol) are added. The reaction is undergone at room temperature for 10 minutes to obtain the catalyst for use.
3. Ethylene Trimerization
500 ml autoclave is heated and vacuumed for 2 hours. After N 2 exchange for several times, ethylene is introduced therein. The temperature is reduced to predetermined temperature. The dehydrated heptane (200 ml) and the catalyst as obtained above are added. Oligomerization is carried out at 100° C. under the pressure of 7.0 MPa. After 10 minutes, the temperature is reduced by ice bath, the pressure is relieved, and the reaction is terminated by 10 wt % acidified alcohol. The results are listed in appended Table 1.
Example 5
1. Preparation of (diphenyl)phosphonitryl(isopropyl)phosphine(diphenyl) ligand
(1) Preparation of N,N-diisopropyldichlorophosphoamide
The process is the same as that in Example 1.
(2) Preparation of Grignard Reagent Phenylmagnesium Bromide
The process is the same as that in Example 1.
(3) Preparation of Diphenyl Phosphorus Chloride
The process is the same as that in Example 1.
(4) Preparation of (diphenyl)phosphonitryl(isopropyl)phosphine(diphenyl)
The process is the same as that in Example 1.
2. Preparation of Catalyst
To a 100 ml reactor with N 2 sufficient exchange, the dehydrated xylene (10 ml), SiO 2 (0.09 mmol), triisobutylaluminium (10 ml), (diphenyl)phosphonitryl(isopropyl)phosphine(diphenyl) (29 mg), CrCl 3 .(THF) 3 (12 mg), and 1,4-dichlorbenzene (0.069 mmol) are added under stirring. The reaction is undergone at room temperature for 5 minutes to obtain the catalyst for use.
3. Ethylene Trimerization
500 ml autoclave is heated and vacuumed for 2 hours. After N 2 exchange for several times, ethylene is introduced therein. The temperature is reduced to predetermined temperature. The dehydrated xylene (200 ml) and the catalyst as obtained above are added. Oligomerization is carried out at 20° C. under the pressure of 5.5 MPa. After 60 minutes, the temperature is reduced by ice bath, the pressure is relieved, and the reaction is terminated by 10 wt % acidified alcohol. The results are listed in appended Table 1.
PRACTICAL APPLICABILITY
This catalyst is used for catalyzing the synthesis of 1-hexene from ethylene trimerization in an inert solvent. The catalyst is prepared by mixing the components of (a)-(e) in a suitable ratio in an ethylene trimerization conventional apparatus in situ under ethylene pressure. And ethylene is introduced into the apparatus continuously so as to get in contact with the catalyst sufficiently, then the ethylene trimerization is performed at the temperature of 30-150° C. under the pressure of 0.5-10.0 MPa for 0.1-4 hours. The catalyst is used to prepare 1-hexene by ethylene trimerization. The catalyst has high catalytic activity and high 1-hexene selectivity. The by-product polyethylene does not stick to the apparatus. The results are listed in appended Table 1.
Appended TABLE 1
Exam-
Exam-
Exam-
Exam-
Exam-
ple 1
ple 2
ple 3
ple 4
ple 5
catalytic activity
5.8
4.1
6.4
5.1
1.6
(g oligomer/
mol Cr · h) _ 10 7
1-butene selectivity
0.3
0.4
0.8
0.4
0.9
(wt %)
1-hexene selectivity
95.1
95.2
95.2
96.3
97.2
(wt %)
polymer (wt %)
0.02
0.05
0.04
0.07
0.02 | A catalyst for synthesizing 1-hexene from ethylene trimerization and its application are provided. Said catalyst consists of (a) the compound containing P and N, (b) electron donor, (c) Cr compound, (d) carrier and (e) accelerator. The molar ratio of (a), (b), (c), (d) and (e) is 0.5-100:0.5-100:1:0.5-10:50-5000. The catalyst is prepared by mixing the components of (a)-(e) in an ethylene trimerization apparatus in situ and ethylene is introduced into the apparatus continuously. The prepared catalyst can be used to synthesize 1-hexene from ethylene trimerization in the inert solvents. The trimerization is performed at 30-150° C. and 0.5-10.0 MPa for 0.1-4 hours. The catalyst has high catalytic activity and high 1-hexene selectivity. During the process of ethylene trimerization, by-product polyethylene does not stick to the apparatus. | 2 |
BACKGROUND OF THE INVENTION
It is well-known to those skilled in the art that bacterial action in sewage (human or animal) produces a complex cascade of products, two of the terminal products of which are hydrogen sulfide and sulfuric acid, the latter of which results from bacterial and/or chemical action on the hydrogen sulfide. The bottom line is that sulfuric acid is produced in quantities that are sufficient to attack the concrete structures so frequently used in handling sewage. The result is the destruction of the concrete component(s), most especially above the water line. In extreme cases, one inch or more of concrete binder can be lost in a year, causing the eventual collapse of the structure. Another problem associated with sulfuric acid attack is that the system becomes more and more porous, allowing dirt and water to infiltrate. This effectively reduces the capacity of the waste treatment system, causing expensive repairs and/or necessitating the addition of plant capacity.
PRIOR ART
Hume (U.S. Pat. No. 6,706,384)
Hume discloses a multilayer system for waste water system rehabilitation, consisting of a spray-applied, multilayer liner, consisting of a primer, first moisture barrier layer, a foam interlayer, and a second moisture barrier layer, or alternatively, a bilayer system consisting of a primer and a hard outer layer. The foam layer, if used, is preferably a polyurea or polyurethane. The patent is rather vague as to the specifics used, but all components are rapid-curing, preferably so rapidly-curing that mixing in the spray gun or preferably in the air between the gun and the wall. The primer is said to possibly be an epoxy, and rigidity is an important part of the whole concept.
In the real world, it takes time for a coating to adequately penetrate concrete. Although the Hume art is creative, the short, essentially zero pot life leaves much to be desired in terms of bonding adequately to the concrete substrate. This problem is general for short-pot life coatings, as will be shown below. As a general rule, polyurea coatings, and other short pot live coatings, contain a multitude of air bubbles, due to the fact that they are spray-applied at high pressures, and air is entrained that cannot escape in the short time the material is semi-fluid. This necessitates very thick coatings, on the order of 100-250 thousandths of an inch.
Also, a rigid material is not always the best choice for a concrete liner. In particular, epoxies have a reputation for being brittle and cracking in service in sewage applications. Therefore, an elastomeric material would provide a more-forgiving coating. The polyurea is said also to be quite rigid.
Another drawback to the Hume invention is the necessity for expensive, sophisticated application equipment. Heated, plural-head sprayers cost tens of thousands of dollars, require multiple trained experts to run, and if the ratio is not correct, a large amount of material can be applied that is useless. The materials are applied at hundreds or thousands of pounds of pressure, representing hazards due to high pressure, and overspray is a major problem, including for personnel that are nearby. Therefore, a more applicator-friendly system is to be desired.
Finally, the use of multiple chemistries is confusing and complicated. A single-chemistry technique, especially one that provides a protective barrier in each and every layer, would be preferable. In this way, any imperfections in any particular layer would be compensated for by the layers above or below, giving an extra measure of protection due to the forgiving nature of the overall system.
Carbonell, et. al. (U.S. Pat. No. 6,127,000)
Carbonell discloses a method and compositions for protecting infrastructure involving dissolving a fluorocarbon polymer in carbon dioxide, and spray applying this coating to the structures to be protected. Presumably this could include manholes and other sewer infrastructure. However, carbon dioxide is capable of displacing oxygen, and is toxic in high concentrations, so presents significant hazards in enclosed environments. Also, the carbon dioxide/fluoropolymer mixture is under high pressure, and represents substantial danger during transport and handling. Fluoropolymers are also under increasing scrutiny due to environmental concerns, with 3M, a major manufacturer, pulling their biggest seller class off the market voluntarily. Finally, both the carrier and fluoropolymers are expensive. Therefore a less-expensive, more acceptable alternative is desirable.
Miller (U.S. Pat. No. 6,056,997)
Miller discloses essentially a long-term disinfectant approach to manhole corrosion inhibition, wherein after cleaning, magnesium hydroxide or magnesium oxide are spray applied to the exposed concrete surface. The high alkalinity inhibits bacterial growth of the type that produces sulfuric acid. The chief advantage of such technology over sodium hydroxide are in the safety and longer-term impact of the magnesium-based technique. However, these magnesium salts are water soluble as well as sodium hydroxide, and will eventually wash off, rendering the surface subject to attack once again. This is especially true for areas where infiltration of outside water occurs, which is a highly-prevalent situation in manholes. Thus, a more-permanent solution is desirable. Similar art is disclosed in U.S. Pat. Nos. 5,620,744 (Huege), 5,7683,748 (Gunderson).
U.S. Pat. No. 5,962,144 (Primeaux)
Primeaux discloses polyurea elastomer systems with improved adhesion to substrates, which is obtained by utilizing castor oil or other primary-hydroxyl-containing hydrophobic chemical and an isocyanate in combination as a primer. The primer system is said to be especially useful on wet substrates, where it will adhere despite the presence of moisture. This primer is said to be especially-useful for improving the adhesion of polyurea elastomer systems. However, the fact that such a primer is necessary indicates the inherent weakness of conventional, short-pot-life polyureas for concrete applications. Also, although the primer is said to function even with the presence of moisture on the surface, moisture is well known to those in the art to cause pinholing in protective liners, and so could not be tolerated in a sewer application. Finally, it would be preferable if every layer of a multilayer system provides barrier properties for the reasons discussed above. Therefore, a better system is desirable.
U.S. Pat. No. 5,795,104 (Schanze)
Schanze discloses a mixture of a silicate solution and a hydrolyzable component such as an orthoester or dialkyl carbonate. The pot life is adjustable, being from a few seconds to 10 minutes. The method of application that Schanze discloses involves sealing the pipe, applying the separate components in a manner wherein they mix in the sealed-off pipe, and after an efficacious curing time, washing the excess away. This system is cumbersome at best, and would be impractical for large pipelines or manholes. Therefore, an improved system for protecting sewer structures is still to be desired.
U.S. Pat. No. 5,415,499 (Hyde-Smith, et al.)
Hyde-Smith discloses a method for repairing existing manholes, consisting of a fast-curing elastomeric material that is spray-applied, preferably on top of a silane-containing primer coat. In addition to the disadvantages of low potlife polyureas mentioned above, this technology suffers from the high toxicity of silanes, which would make working with the primer dangerous. Therefore, a more user-friendly system is desirable.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to an improved method of protecting concrete sewer pipe, manholes, lift stations, pump stations, wet wells, sewage treatment plant components, and septic tanks and/or septic tank components involving a polyurea coating system. There are a plurality of coats applied, and the pot life of all of them is such that they may be brush- or roller-applied, as well as sprayed. The basic chemistry of all of the layers is the same, so all of the layers provide barrier protection of the concrete, making the whole system forgiving to minor application errors. The primer also has time to soak into the concrete, forming a coating that is integral to the concrete, greatly inhibiting delamination of the coating.
The method comprises coating said concrete items by rolling, spraying, or brushing on a coating system consisting essentially of:
1. A primer coat, consisting essentially of an “A” component which is a mixture of:
a. At least one amino-terminated prepolymer of the structure (NHR)n[X]x[Y]y, wherein N is a nitrogen atom, H is a hydrogen atom, R is an alkyl, aryl or alkylaryl radical, X and Y are interchangeably propylene glycol- or tetramethylene glycol units, x and y are integers from 0 to 1000, with the exception that the number of tetramethylene glycol units is never zero for all prepolymers, i.e. at least one prepolymer is an amino-terminated polytetramethylene glycol (“PTMEG”) oligomer, with at least one tetramethylene glycol unit in it's structure, the total amount of such prepolymer(s) being from about 1 to about 30 percent by weight of the total formulation, and wherein the particular prepolymer components are chosen and present in such a composition ratio so as to render the working pot life of the combined A/B mixture at least 15 minutes, and
b. At least one solvent chosen from the group containing lower ketone solvents (acetone, methyl ethyl ketone, etc., up to around a 10-carbon ketone), lower ester solvents (propylene glycol methyl ether acetate, methyl acetate, ethyl acetate, etc., up to around a 15-carbon ester solvent), aromatic, aliphatic, and alkyl-aryl hydrocarbons, said solvents in sum comprising from about 70 to about 95 percent of the A component, and
c. Other optional additives such as thickeners, opacifying and/or coloring agents, and
2. An intermediate coat, consisting essentially of: an “A” component which is a mixture of:
a. At least one amino-terminated prepolymer of the structure (NHR)n[X]x[Y]y, wherein N is a nitrogen atom, H is a hydrogen atom, R is an alkyl, aryl or alkylaryl radical, X and Y are interchangeably propylene glycol- or tetramethylene glycol units, x and y are integers from 0 to 1000, with the exception that the number of tetramethylene glycol units is never zero for all prepolymers, i.e. at least one prepolymer is an amino-terminated polytetramethylene glycol (“PTMEG”) oligomer, with at least one tetramethylene glycol unit in it's structure, the total amount of such prepolymer(s) being from about 20 to about 90 percent by weight of the total formulation, and wherein the particular prepolymer components are chosen and present in such a composition ratio so as to render the working pot life of the combined A/B mixture at least 15 minutes,
b. At least one solvent chosen from the group containing lower ketone solvents (acetone, methyl ethyl ketone, etc., up to around a 10-carbon ketone), lower ester solvents (propylene glycol methyl ether acetate, methyl acetate, ethyl acetate, etc., up to around a 15-carbon ester solvent), aromatic, aliphatic, and alkyl-aryl hydrocarbons, said solvent (mixture) comprising from about zero to about 40 percent by weight of the total A component, and
c. A filler or fillers, being at least one chosen from the group containing ceramic microspheres, glass microspheres, plastic microspheres, mica, clays, barytes, molybdenum sulfide, iron oxide, titanium dioxide and/or other metal oxides, such filler or fillers comprising from about 5 to about 80 percent by volume of the whole “A” component,
d. A thickener or thickeners, of such type and amount such that the final formulation, exhibits excellent vertical “cling”, yielding a dry film of about 40 thousandths of an inch or more, and
e. Other optional additives such as opacifying and/or coloring agents, defoamers and the like, and
Wherein said intermediate coat “A” component is admixed with an appropriate isocyanate optionally dissolved in a solvent (as described above) in an equivalent ratio of from about 1 to about 10 with respect to the prepolymer component, and which combined A-component/isocyanate combined intermediate coat may be applied multiple times to build up heavier final thicknesses of the coating system, and
3. A topcoat consisting essentially of an “A” component which is a mixture of:
a. At least one amino-terminated prepolymer of the structure (NHR)n[X]x[Y]y, wherein N is a nitrogen atom, H is a hydrogen atom, R is an alkyl, aryl or alkylaryl radical, X and Y are interchangeably propylene glycol- or tetramethylene glycol units, x and y are integers from 0 to 1000, with the exception that the number of tetramethylene glycol units is never zero for all prepolymers, i.e. at least one prepolymer is an amino-terminated polytetramethylene glycol (“PTMEG”) oligomer, with at least one tetramethylene glycol unit in it's structure, the total amount of such prepolymer(s) being from about 10 to about 90 percent by weight of the total formulation, and wherein the particular prepolymer components are chosen and present in such a composition ratio so as to render the working pot life of the combined A/B mixture at least 15 minutes,
b. At least one solvent chosen from the group containing lower ketone solvents (acetone, methyl ethyl ketone, etc., up to around a 10-carbon ketone), lower ester solvents (propylene glycol methyl ether acetate, methyl acetate, ethyl acetate, etc., up to around a 15-carbon ester solvent), aromatic, aliphatic, and alkyl-aryl hydrocarbons, said solvents in sum comprising from about 10 to about 90 percent of the A component, and
c. A filler or fillers, being at least one chosen from the group containing ceramic microspheres, glass microspheres, plastic microspheres, mica, clays, barytes, molybdenum sulfide, iron-, titanium- or other metal oxides, said filler or fillers comprising from about 10 to about 80 percent by volume of the final “A” component,
d. Other optional additives such as thickeners, opacifying and/or coloring agents, and
Wherein said top coat “A” component is admixed with an appropriate isocyanate optionally dissolved in a solvent as described above in an equivalent ratio of from about 1 to about 10 with respect to the prepolymer component, such that the topcoat thickness is from about 5 to about 20 thousandths of an inch when dry.
The prepolymer is either a single component or a blend. An example of polyurea prepolymers that find utility in the present invention are the “Versalink” polyether polyamines manufactured by Air products. The backbone of these oligomeric amines are poly(tetrahydrofuran), also known as polytetramethylene glycol (“PTMEG”). The endcaps are typically aminobenzoic acid esters of the PTMEG backbone. These materials make polymers upon addition of traditional isocyanates, such as those of methylene-bis-phenylisocyanate (“MDI”). The polymers are excellent water barriers, and the pot life, which depends on the solvent concentration as well as that of the other additives and the particular choice of isocyanate, is typically never less than 15 minutes at ambient temperatures less than about 100 degrees F., unless a catalyst is used. Examples of the Versalink prepolymers that find utility in the present invention include, but are not limited to, Versalink P-250, P-650, P-1000, P-2000, and P-3000. Other PTMEG-based amino-terminated prepolymers would also find utility in the present invention, provided that alone or in combination with other amino-terminated prepolymers, the pot life is sufficient to allow excellent adhesion to concrete and/or other layers of a coating system. The amount of such prepolymers in the particular coating component depends on whether the coating is a primer, intermediate or top coat. For a primer, the best concentration is 5-30 percent by weight, with most of the balance being solvent.
It has been surprisingly found that aliphatic amines, diamines and triamines also find utility in the instant invention, although not in high concentrations compared to the Veralink PTMEG-based aminobenzoate-terminated prepolymers. These are exemplified by the Jeffamine and XTJ prepolymers sold by the Huntsman Corporation. These are generally based on polypropylene glycols of various molecular weights that are then reacted with ammonia to form amino-terminated polypropylene glycols. Alone, these materials react virtually instantaneously with isocyanates, necessitating the complex, plural-head sprayers discussed above to apply them. However, surprisingly, it has been found that these materials can be admixed in with the PTMEG-based aminobenzoates discussed above, and provided their concentration is not overly high, a good pot life can nonetheless be obtained. The concentration of the material allowable depends on the rest of the formulation as well as the exact type of aliphatic amine or polyamine. As a general rule, no more than an 80/20 mixture of PTMEG-based aminobenzoate/aliphatic amine can be utilized for pot lives of 15 minutes or greater, although higher concentrations of aliphatic amines are potentially useful as well. It is of course understood by those skilled in the art that other aliphatic amines or polyamines will find utility in the instant invention.
Solvents that find utility in the instant invention are typically those compatible with the prepolymer or prepolymer blend. The exact nature of the solvent or solvent blend that is chosen depends on the nature of the coating and the desired cure time, etc. Solvents that find utility in the present invention include, but are not limited to: acetone, methyl ethyl ketone or other ketone solvents with less than 10 carbon atoms in their carbon skeleton, propylene glycol methyl ether acetate, ethylene glycol methyl ether acetate, and other alkyl ether acetates with less than 20 carbon atoms in their carbon skeleton, ethers such as diethyl ether, tetrahydrofuran, and other ether solvents with less than about 12 carbon atoms in their carbon skeleton, benzene, toluene, xylene, and other aromatic-based solvents with less than about 12 carbon atoms in their carbon skeletons. This list is representative, not exhaustive.
The coatings of the instant invention are all two-component coatings, with an “A” component being mixed with a hardener or “B” component in the field just prior to application. The hardeners of the instant invention are isocyanates with at least two isocyanate groups per molecule. The exact choice of isocyanate is determined by the desired parameters for the formulation, such as cost, pot life, compatibility with solvents and other formulation (A or B side) components, etc. Such isocyanates are well-known to those skilled in the art. Examples include, but are not exclusively: methylene-bis-phenyl isocyanate (MDI) or polymers or addition products thereof, toluene di-isocyanate (“TDI”) or polymers or addition products thereof, as well as other aromatic isocyanates or polyisocyanates, aliphatic isocyanates such as hexamethylene-di-isocyanate (“HDI”), or dimers, trimers, and other addition products thereof, isophorone di-isocyanate (“IPDI”), or dimers, trimers, and other addition products thereof, or alternatively pre-polymers made from blending a polyether polyol and an isocyanate, or mixtures or combinations of these. The exact quantity of isocyanate in the B side formulation depends on the choice of solvent and nature of the isocyanate or isocyanates. Typically, the isocyanate is present from about 60 to about 100% by weight in the “B” side formulation. The exact amount of “B” side formulation mixed with “A” side formulation depends on the concentration of reactive components in the “A” side formulation, as well as desired stiffness, pot life, and other similar considerations known to those skilled in the art. Generally, the equivalent ratio of reactive components in the “A” and “B” sides is close to 1.0, but ratios up to 10 to 1 for the isocyanate equivalents to reactive “A” side components are potentially useful. These higher ratios would lead to “moisture” curing coatings, and have long pot lives, although the moisture cure aspect can lead to foaming during curing. Therefore, more preferable A/B equivalent ratios are between 1:1 and 1:2 (pre-polymer/isocyanate).
For building up thicknesses of coatings, and to reduce the costs of the overall coatings, fillers are typically added to the “A” side. Conventional fillers utilized in coatings find utility in this method as well, except that the fillers should not detract from the water-resistance of the coating, and should be compatible with the prepolymer and/or the final polymer. Those skilled in the art will know of many possible fillers that could find utility in the present invention. Examples of fillers that find utility in the instant invention include, but are not limited to: hollow microspheres such as those made of ceramic, glass or plastic, mica or other platy minerals, clays, such as bentonites, hectorites, or modified clays such as those made by adding long-chain cationic amines to clays, barites, magnesium aluminosilicates, crushed glass, or silica.
Other potential additives are known to those skilled in the art. Pigments or pigment dispersions are useful to provide aesthetic appeal, as well as provide ready visibility of incomplete coating, thickeners are used to reduce the tendency of the applied, uncured coating to sag off. Water-scavenging materials can make the “A” side foam less when mixed with the “B” side. Defoamers can eliminate foam that forms during the mixing and/or application process. The exact nature and concentration of these additives are found by experimentation processes known to those skilled in the art.
EXAMPLE
A coating system was prepared by mixing the following proportions (W/W) of ingredients utilizing conventional (low-shear) mixing equipment:
Parts
by weight
Material
PRIMER
13.9
Versalink P-1000
3.1
Jeffamine D-2000
33
Propylene glycol methyl ether acetate
50
acetone
INTERMEDIATE COAT
60.1
Versalink P-1000
3
Huntsman XTJ-510
26.5
Ceramic microspheres
0.1
Modaflow flow control agent
0.6
Aerosil R-972 fumed, hydrophobic silica
1
Cravallac PA4X20 thickener
0.5
Zoldine MS-Plus drying agent
8.1
acetone
TOP COAT
40.5
Versalink P-1000
40.5
Mica “3X”
1.7
Mixture of Degussa 844 Phthalo blue and titanium white tint
16.2
Propylene glycol methyl ether acetate
HARDENER
79
Isonate Polymeric MDI
21
Propylene glycol methyl ether acetate
The hardener was mixed with the various coating “A” components in the portions below (all by volume) The approximate pot lives at 80 degrees F. were all greater than 15 minutes.
PRIMER
5 gallons to 1 quart hardener
INTERMEDIATE COAT
1 gallon to 1 quart hardener
TOP COAT
1 gallon to 1 quart hardener
A. The three coats were used to coat a manhole that had suffered significant damage due to corrosion, in Garner, N.C. After cleaning it thoroughly with high-pressure water, the surface was dried, but not re-concreted. The primer was spread at a rate of approximately 100 square feet per gallon, in multiple passes, using brushes and rollers. After approximately 45 minutes, the intermediate coat was applied, in one pass, at an approximate rate of 20-40 square feet per gallon. The top coat was then applied about 1 hour later, when the intermediate coat was dry to the touch, in one pass, with brush and/or roller touchup, at a rate of approximately 100-150 square feet per gallon. The resultant product had sufficient integrity to pass a “holiday test” at 10,000 volts with no spots causing sparking in the interior of the manhole, away from the metal rim or stairs.
B. The three coats were used to coat the pieces of a manhole that had not yet been installed. After acid etching with hydrochloric acid solution, and then cleaning it thoroughly with high-pressure water, the surface was allowed to dry. The primer was spread at a rate of approximately 100 square feet per gallon, in multiple passes, using brushes and rollers. After approximately 45 minutes, the intermediate coat was applied, in one pass, at an approximate rate of 20-40 square feet per gallon. The top coat was then applied about 1 hour later, when the intermediate coat was dry to the touch, in one pass, with brush and/or roller touchup, at a rate of approximately 100-150 square feet per gallon The resultant product had sufficient integrity to pass a “holiday test” at 10,000 volts with no spots causing sparking in the interior of the manhole, away from the metal rim or stairs. | This invention relates to a method of protecting concrete sewer pipe, manholes, lift stations, pump stations, wet wells, sewage treatment plant components, and septic tanks and/or septic tank components comprising coating said concrete items by rolling, spraying, or brushing on a coating system consisting essentially of a primer, intermediate coat and topcoat. Each coat is a polymeric coating prepared in situ by combining a hardener with a prepolymer formulation. The pepolymer is an amine-containing material, resulting in a polyurea-based coating. The chief advantages of the coating are that it can be applied utilizing conventional, simple equipment, and the increased drying time allows for excellent adhesion on the substrate. Also, it is a tough elastomeric material resistant to attack by water or the sulfuric acid microbial metabolic end-product. | 2 |
FIELD OF THE INVENTION
This invention relates to fluid valves. More particularly, it relates to a valve which can be used in systems designed to measure extremely small pressure changes, volume changes and flow differences in high pressure fluids.
BACKGROUND OF THE INVENTION
It is necessary in certain types of laboratory analysis work to accurately measure pressure changes, volume changes and fluid flow in a high fluid pressure system. In fine core analyses conducted in the oil industry, for example, the system pressures are commonly in the order of 10,000 psi, while the changes in pressure, volume and flow which must be measured are very small. Pressure changes are measured to a fraction of a psi, volume changes are measured in thousandths of a cc and flow changes are measured in thousandths of a cc per minute.
Valves currently available suffer from one or more problems. In most cases the internal volume of the valve changes upon opening and closing of the valve. In other words, the structure of the movable component of the valve increases or decreases the volume of the flow path through the valve depending upon whether the valve is open or closed. As a result, the pressure of the fluid and the total volume in the system changes. Since extremely small changes in pressure and volume can be significant, even small changes in the volume of the system can cause erroneous readings, leading to erroneous conclusions about the core sample.
In addition, most valves available for use in such systems do not give flexibility of operation when incorporated in a multiple valve. In a three-way valve, for example, it can be desirable to be able to close both outlets or open them both, which is not possible with currently available valves. Further, most valves used in such systems are quite expensive.
It would therefore be desirable, in the measurement of small fluctuations in pressure, volume and flow in a high pressure fluid system, to use a valve that maintains a constant internal volume so as not to produce false pressure readings. It would also be desirable that such a valve be economical and capable of a full range of settings when used in a multi-valve arrangement.
SUMMARY OF THE INVENTION
This invention provides a valve comprising a movable member and a fixed member, one of the members including a fluid passageway terminating in an annular valve seat and the other member comprising a closure element adapted to engage the valve seat to stop fluid flow through the passageway. Means are provided for moving the movable valve member to cause the closure element to be either engaged with the valve seat or spaced therefrom. The fluid path includes a first fluid chamber adjacent the valve seat and a second fluid chamber spaced from the first chamber. The movable member is designed to move into the first fluid chamber as the valve is closed to decrease the volume of the first fluid chamber. In addition, means are provided for increasing the volume of the second fluid chamber as the valve is closed by an amount corresponding to the amount by which the first fluid chamber is decreased. The internal volume of the valve thus remains substantially the same during activation of the valve.
Although any suitable means for moving the movable valve member may be employed, a piston is the preferred means because it fits well into a computer controlled system. The piston contains an aperture in which the movable valve member is located for movement with the piston. The fluid path of the valve would thus extend through the piston.
The valve can be designed so that the movable member comprises either the valve closure element or the fluid passageway which contains the valve seat, or it can be designed as a combination of the two. In one embodiment, the movable valve member comprises a body portion containing a bore which slidably receives opposed tubular portions leading to the inlet and outlet of the valve. The closure element is located within the body portion between the ends of the tubular portions, one of which contains the valve seat. The volume of the first fluid chamber is changed by movement of the closure element with respect to the tubular element containing the valve seat, and the volume of the second fluid chamber is changed by movement of the closure element with respect to the other tubular portion, whereby movement of the closure element toward the valve seat decreases the volume of the first chamber and increases the volume of the second chamber.
In another embodiment the movable valve member comprises a tubular portion containing the fluid passageway which carries the valve seat. The tubular portion is slidably mounted in aligned bores leading to the inlet and outlet. The volumes of the first and second chambers are changed by movement of the tubular portion with respect to the fixed closure element, whereby movement of the tubular portion toward the closure element decreases the volume of the first chamber and increases the volume of the second chamber.
In addition, a third embodiment which combines features of the two embodiments just described can be utilized.
Because of the valve construction, the surfaces of the valve exposed to fluid are kept to a minimum, thereby minimizing the use of expensive corrosion resistant materials. Also, the valve design allows it to be incorporated in multi-valve arrangements wherein each valve can be set in open or closed condition as desired.
Other features an aspects of the invention, as well as other benefits, will readily be ascertained from the more detailed description of the invention which follows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal sectional view of a two-way valve in open condition, illustrating one embodiment of the invention;
FIG. 2 is an enlarged longitudinal sectional view of the movable body member containing the closure or sealing element;
FIG. 3 is a transverse sectional view of the sealing element taken on line 3--3 of FIG. 2;
FIG. 4 is a partial pictorial view of the movable body member illustrated in FIGS. 2 and 3;
FIG. 5 is a partial longitudinal sectional view of the valve shown in FIG. 1, but showing the valve in closed condition;
FIG. 6 is an enlarged longitudinal sectional view similar to that of FIG. 2, but showing the valve in closed condition;
FIG. 7 is a longitudinal sectional view of a different two-way valve in open condition, illustrating a second embodiment of the invention;
FIG. 8 is a partial longitudinal sectional view of the valve shown in FIG. 7, but showing the valve in closed condition;
FIG. 9 is a longitudinal sectional view of another two-way valve in open condition, illustrating a third embodiment of the invention;
FIG. 10 is a pictorial view showing the exterior of a typical three-way valve incorporating the valve of the present invention; and
FIG. 11 is a longitudinal sectional view of a three-way valve incorporating the movable valve body design of FIG. 1;
FIG. 12 is a pictorial view showing the exterior of a five-valve configuration incorporating the valve of the present invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1, a valve 10 is comprised of a main body 12 consisting of cylindrical portions 14 and 16 connected to each other by threads 18. The cylindrical portions 14 and 16 include end portions 20 and 22, respectively, which extend radially inwardly toward end sections 24 and 26 and are connected thereto by threaded connections 28 and 30. Extending from the central portions of the end sections 24 and 26 are ports 32 and 34 adapted to receive threaded fluid connectors, not shown. The ports 32 and 34 are connected to bores 36 and 38, respectively, which extend through tubular extensions 40 and 42. The tubular extensions 40 and 42, which are of the same cross-sectional dimensions, also extend centrally of the end sections 24 and 26, and the bores therein are axially aligned with each other.
The enclosure formed by the cylindrical portions 14 and 16, the end portions 20 and 22, and the end sections 24 and 26 comprises a chamber 44 in which a piston 46 is mounted for reciprocal movement. The piston 46 comprises two halves 48 and 50 connected to each other by threaded connection 52. Each half piston section contains a peripheral groove 54 in which an O-ring 56 is seated. The end portions 20 and 22 contain ports 58 and 60 connected to bores 62 and 64 which permit pressurized fluid, such as air, to be admitted to the chamber 44 to move the piston 46 in the chamber toward and away from the bores 36 and 38. Each piston half 48 and 50 contains a centrally located bore which meets with the other bore to form a centrally located cavity 66 in which a cylindrical body 68 is fitted.
As shown generally in FIG. 1, and in more detail in FIG. 2, the cylindrical body 68 includes a relatively short axial bore 70 intermediate the ends of the body 68, the bore 70 being dimensioned so as to slidably receive the tubular extension 40. The rest of the body is counterbored as at 74 to a larger diameter. This arrangement enables O-ring 76 to be installed as part of an assembly in which the O-ring is sandwiched between back-up rings 78 at the left counterbore 74, wherein the inner back-up ring 78 abuts a shoulder 80 connecting the bore 70 and the left counterbore 74. A similar assembly including O-ring 82 and back-up rings 84 is installed in the right counterbore at the other end of the cylindrical body, but in this case the inner back-up ring 84 abuts one end of a retaining ring 86. The other end of the retaining ring 86 abuts one end of a sealing plug 88 which is sandwiched between the retaining ring 86 and the shoulder 90 connecting the bore 70 and the right counterbore 74.
As shown in FIGS. 2, 3 and 4, the sealing plug 88 comprises a cylindrical body from which a conical sealing element 92 extends. The sealing element is located centrally of the cylindrical body and is aligned with the bore 38 of tubular extension 42, being adapted to seat in the end portion of tubular extension 42. The slope of the cone is similar to the slope of the seat 94 at the end of the tubular extension 42 so as to form a fluid tight seal when the cone engages the end of the tubular extension. The opposite end of the sealing plug includes a centrally located dished portion forming a recess 96. Bores 98 in the sealing plug 88 provide fluid passages between the recess 96 and the opposite end of the sealing plug adjacent the base of the cone 92.
Referring to FIGS. 1 and 2, either port 32 or 34 may function as the inlet while the other port would function as the outlet. Assuming for the sake of illustrating the operation of the valve that system fluid is introduced into port 34, it will flow through the bore 38 and into a chamber 100 defined by the cone 92, the end portions of the sealing plug 88 surrounding the cone, the end of the tubular extension 42 and the surrounding portions of the retaining ring 86. For purpose of discussion and according to the terminology used in the claims, this chamber will be referred to as the first fluid chamber. The system fluid will then flow out the first fluid chamber, through the bores 98, and into a second fluid chamber 101 defined by the recess 96 of the sealing plug, the end of the tubular extension 40 and the surrounding portions of the bore 70. The fluid will then continue through the bore 36 and out the outlet port 32.
To close the valve, pressurized air would be introduced into the piston chamber 44 through port 58. The air introduced would remain on the left side of the piston as seen in FIG. 1, due to the sealing action of the left O-ring 56. The force of the air pressure moves the piston to the right, exhausting air from the right side of the piston chamber through the port 60. As the piston is moved toward the right, the cylindrical body 68 is moved with it, causing the conical sealing element 92 to engage the valve seat 94 at the end of the tubular extension 42 to close the fluid path at the end of the tubular extension. The positions of the various elements at this stage are shown in FIGS. 5 and 6.
It can be seen, particularly by comparing FIGS. 2 and 6, that the movement to the right by the cylindrical body 68 causes the sealing plug 88 to move away from the fixed end of the tubular extension 40, thus increasing the volume of the second fluid chamber 101. The same movement causes the conical sealing element 92 to move closer to, and eventually engage, the seat 94 at the fixed end of the tubular extension 42, thus decreasing the volume of the first fluid chamber 100. By making the outside and inside diameters of the tubular extension 40 the same as the outside and inside diameters of the tubular extension 42, the amount that the volume of the first fluid chamber 100 has been decreased at any moment during movement of the sealing plug 88 and the conical sealing element 92 in a direction toward the end of the tubular extension 42 will be equal to the amount that the volume of the second fluid chamber 101 has been increased. Therefore, the internal volume of the valve at any moment, whether the sealing member is stationary or moving, remains the same.
In the arrangement described, the movable sealing assembly slides over the tubular extensions of the end sections of the valve body. The design can be reversed, however, to make the movable component slide within bores in the end sections. Referring to FIG. 7, the valve 102 illustrates such an arrangement. A main body portion 103, generally similar to the body 12 of the FIG. 1 design, is connected to end sections 104 and 106 which contain ports 108 and 110, respectively. A piston 112 is positioned in the chamber 114 for reciprocal movement therein, and O-rings 116 and 118 seal the chamber to allow pressurized air to enter and exhaust from ports 120 and 122.
Still referring to FIG. 7, instead of tubular portions extending toward each other from the end sections, as in the first embodiment described, the end sections 104 and 106 contain bores or sockets for receiving the end portions of tube 124. Thus end section 104 contains bore 125 and counterbore 126, which are similar in function to the bore 70 and counterbore 74 in the first embodiment. End section 106 contains bore 127 for receiving a sealing plug and retaining ring arrangement similar to the sealing plug 88 and retaining ring 86 previously described. The tube 124, which is of constant cross-sectional dimensions throughout its length, extends into the end sections 104 and 106 through centrally located openings 128 in the main body portion 103. The tube 124 is connected to the piston 112 for movement therewith by any suitable means, such as by brazing, indicated for purpose of illustration by reference numeral 130. A fixed conical sealing element 132 is mounted in the bore 126 in the end section 106 in axial alignment with the tube 124 so that the adjacent end of the tube can be moved into engagement with the element 132. The end of the tube functions as a valve seat, as in the arrangement of FIG. 1, so that engagement with the sealing element 132 stops fluid flow through the tube. The sealing element 132 may be part of a sealing plug 134 similar to the sealing module 86 of FIGS. 1-5.
As in the first embodiment, this embodiment has a first fluid chamber 136, defined by the same type of structure which defines the first fluid chamber 100 in the first embodiment, and a second fluid chamber 138, which is defined by the end of the tube 124, and the end and surrounding portions of the bore 125 in the end section 104. In operation, when the piston 112 is actuated to move from the open valve position in FIG. 7 to the closed valve position in FIG. 8, the first fluid chamber 136 is reduced in volume by an amount similar to the amount that the second fluid chamber 138 is increased in volume. This is due to the inside and outside diameters of the end portions of the tube 124 being respectively equal. The total fluid volume of the valve thus remains unchanged as in the embodiment of FIGS. 1-5.
Another feature of the invention is illustrated in FIG. 7, wherein O-rings 140 engage the surface of inwardly directed cylindrical stubs extending from the end portions of the valve body 102 to seal off the annular space adjacent the movable tube 128. A bore 142 in the piston 112 connects the annular space on opposite sides of the piston, and a bore 144 connects the bore 142 with the annular space between the periphery of the piston and the interior cylindrical surface of the valve body. A bore 146 in the valve body completes the fluid path. This arrangement provides a flow path for system fluid which may leak into the piston chamber. Such fluid would thus be prevented by this arrangement from entering the portions of the piston chamber containing pressurized air. Although described in connection with the embodiment of FIGS. 7 and 8, it is obvious that a similar leak path could be provided in the first embodiment by altering the shape of the end sections and the piston.
Referring to FIG. 9, a third embodiment is illustrated by the valve 150 which comprises a main body portion 152, end sections 154 and 156, and a piston 158. The design of this embodiment combines certain features of the first two embodiments by providing a movable tubular portion 160 and co-acting fixed conical sealing element 162, as in the FIG. 7 arrangement, and a tubular extension 164 fitting into a socket or bore 166 in the piston, as in the FIG. 1 arrangement. The chamber 168, similar to the chamber 136 in the FIG. 7 arrangement, is the first chamber and the chamber 170, similar to the chamber 101 in the FIG. 1 arrangement, is the second chamber.
The embodiment of FIG. 9 functions in the same general manner as the other embodiments, with the piston 158 causing the seat in the end of the tubular portion 160 to engage or disengage the sealing element 162 in order to close or open the valve. Due to the inside and outside diameters of the end portions of tubes 160 and 164 being respectively equal, the chambers 168 and 170 correspondingly decrease or increase in volume so as to maintain the internal volume of the valve constant at all times. As in the arrangement of FIG. 7, a leak path could also be provided in this design.
FIG. 11 shows a typical three-way valve utilizing the valve design of the present invention. In this arrangement fluid is admitted through the inlet 180 in central body portion 182, from which it flows through bore 184 into valves 186 and 188. These valves may be of any of the designs of the various embodiments of the invention and, depending on the position of the pistons 190 and 192 thereof, will either permit or prevent flow through the outlets 194 and 196. It will readily be seen that the design of the invention permits the valves 186 and 188 to be operated in any desired sequence so that either or both valves can be opened or closed at any time independent of the operation of the other.
A three-way valve such as that shown in FIG. 11 would typically appear as in FIG. 10, wherein the valves 186 and 188 may be formed flush with the body portion 182 to provide an overall valve assembly which is convenient to handle. The valves in this case are shown with air line attachment assemblies 198 leading into valve 186 and attachment assemblies 199 leading into valve 188.
A number of valves may be connected together to form multi-valve arrangements. For example, in FIG. 12 five valves 200, 202, 204, 206 and 208 are shown connected to a common inlet 210 in a typical modular arrangement. It will be understood that any number of valves may be strung together in connection with a common inlet or outlet as required to provide for controlled multiple valve operation.
While various designs have been described, the final choice of design may well be dictated by the ease and cost of assembly. In this connection, the piston, the valve body and the sealing assemblies have been illustrated as being comprised of components secured together by threaded connections which permit the various parts to be readily assembled. Since each embodiment described operates on the same basic principles, each will provide the same function and can be used interchangeably if desired.
Although the sealing element has been illustrated as a conical element, it could just as well be any other shape, such as flat or arcuate, which will effectively engage the valve seat and provide the desired sealing function. This element may be comprised of any suitable material such as plastic, metal or rubber, as long as it functions in the desired manner and is resistant to the effects of corrosive fluids in the system.
Although the preferred means for moving the movable sealing elements is a piston because its operation lends itself to computer control and because it is fast acting, other means such as solenoids or even manually controlled movement of the sealing assembly may be employed.
Although the sealing plug and retaining ring assembly shown in the drawings is preferred because the parts can be replaced if worn and because it lends itself to easy assembly in the valve, it will be appreciated that there are other sealing element designs which may or may not involve a sealing plug and retaining ring arrangement of the type described. Similarly, the design of the first and second fluid chambers, whose volumes change so as to maintain the internal volume of the valve constant, need not be specifically as shown so long as the relationship between the two enables a constant valve volume to be maintained.
It should now be understood that the invention is not necessarily limited to all the specific details of the preferred embodiments but that changes to certain features of the preferred embodiment which do not alter the overall basic function and concept of the invention may be made by those skilled in the art without departing from the spirit and scope of the invention, as defined in the appended claims. | A high pressure fluid valve includes a tubular portion with a valve seat on its end and a closure element for engaging the valve seat. A piston carries either the tubular portion or the closure element as a movable valve member, with the other being fixed. A first fluid chamber is provided adjacent the valve seat and a second fluid chamber is spaced therefrom adjacent the other end of the movable valve member. When the movable valve member is actuated, one of the fluid chambers increases in volume by the same amount that the other decreases in volume, thereby maintaining the internal volume of the valve constant. | 5 |
BACKGROUND OF THE INVENTION
Apartments and other large buildings are often provided with so-called zone heating and cooling systems wherein a building system is provided with pressurized hot water or coolant. Individual rooms or zones are thermostatically controlled and individual valves responsive to the thermostat are placed in the lines leading to the rooms or zones to allow control of the fluid to the radiators in each area. Inevitably, as with all mechanical devices, these zone control valves require servicing, that is replacement or repair of these seals therein. Heretofore this has required generally shutting down the whole system in order to repair or replace one valve. This can be quite inefficient and also leaves the whole building without heating or cooling while one area is being serviced.
U.S. Pat. Nos. 3,275,023, 4,127,141, and 2,746,470 all deal with the problems of servicing pressurized valves. However, none of these prior art patents are suitable for the type of servicing described above.
It is, therefore, an object to this invention to provide a device which will permit the servicing of a valve under pressure. It is also an object to this invention to provide such an apparatus and method as to permit the servicing to be accomplished quickly and efficiently and which requires a minimum of space due to the confined nature of the areas in which such valves are often located.
SUMMARY OF THE INVENTION
In the instant invention, the motor for the zone control is removed and the tool valve is fastened in its place on top of the zone control valve. A puller mechanism is then inserted into the tool valve, the puller mechanism having a number of tangs which snappingly engage into a groove found in the top of the zone control valve plug stem. A collar is then placed over a portion of the pulling mechanism so that only the handle of the pulling mechanism extends out of the tool valve. The handle has been drawn upwardly pulling the puller and the valve plug into the core of the tool valve. The core of the tool valve then is rotated to a position isolating it from the heating system. At that point the collar may be removed and the plug removed for repair and/or replacement; reassembly takes place in the reverse of the above description.
These and other objects of my invention will become readily apparent as the following description is read in conjunction with the accompanying drawings wherein like reference numerals are used to refer to the several views.
DESCRIPTION OF THE DRAWING FIGURES
FIG. 1 is an exploded perspective view of the invention.
FIG. 2 is a vertical sectional view showing the initial stages of valve removal.
FIG. 3 is a sectional view taken along the same section as FIG. 2 and showing the tool valve in the isolation position.
FIG. 4 is a sectional view taken along lines 4--4 of FIG. 2.
FIG. 5 is a perspective view showing the tool in conjunction with the retaining clip for reinstallation.
FIG. 6 is an exterior view showing the retaining clip.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Turning now to the drawings, FIG. 1 shows generally a valve pulling device 10 and an exploded view. Device 10 is designed to be attached to a zone control valve 12 (or any other similar type of valve which is normally under pressure). Valve 12 has, generally, a pair of ears 14 with holes therein upon which a thermostatically controlled electric motor is normally mounted. For servicing the valve, this motor is removed. Valve 12 has a through passage 16 which may be closed by rotation of valve plug 20 which is located in a cylindrical bore 18. A seal 22 is used to prevent leakage, and it is this seal which generally requires replacing after a period of time and service. A stem 24 is located on top of core 20, stem 24 typically having a groove 26 located about its circumference. It should be emphasized that the parts described above are all present in a vast majority of zone control valves being used today. Thus the instant invention is suited for servicing most of those valves.
The tool 10 is comprised of a tool valve body 34 having a rotatable tool valve core 28 located therein, tool valve core 28 having a cylindrical bore 30 therethrough. Bore 30 is sized to accommodate the outer diameter of zone control valve plug 20. The upper end of bore 30 is provided with threads 32 which meetingly engage with collar 44 which has a corresponding inner diameter and upper lip 48 which has a bore 50 therein sized to accommodate handle 54 as described more fully hereinafter. Housing 34 has stops 36 and 38 located therein to control and limit rotation of tool valve core 28 therein; these stops limiting travel to the position shown in FIGS. 2 and 3. Slots 40 are provided in tool valve body 34 for attachment via bolts 41 to ears 14 of zone control valve 12.
A grease fitting 42 is provided in the side of housing 34 to enable grease to be injected and provide a sealing and lubricating capability between tool valve core 28 and body 34. As noted previously, collar 44 has threads 46 at the lower end thereof for threading engagement with threads 32 of plug 28.
A pulling device, generally 52, is comprised of a handle 54 designed for threading engagement with the upper end 56a of U-joint 56. Attached to the lower end of U-joint 56 are a plurality of fingers 58 having tangs 60 on the inner side thereof designed for snap fitting engagement with groove 26 of stem 24.
A retaining flange 62, the use of which is described hereinafter, is formed of a U-shaped piece having an upper plate 64 and a lower plate 66. A slot 68 located in upper plate 64 is sized to correspond approximately to the diameter of stem 24 of core 20. The lower slot 70 located in lower plate 66 is sized to fit beneath ears 14 and retain flange 62 to valve 12.
OPERATION OF THE INVENTION
In order to repair a zone control valve 12 such as that shown, a thermostatically controlled motor (not shown) is removed and tool valve body 34 bolted thereon with bolts 41 passing through slots 40 into ears 14 of zone control valve 12. It is desirable to have some sort of method of sealing the tool valve body 34 to the zone control valve 12, and towards this end any number of conventional means may be used. An O-ring may be located in the bottom surface of tool valve body 34 or alternatively, duct putty may be placed on the bottom of body 34 to effect a seal. The use of the duct putty may often be desirable in conjunction with the O-ring where the zone control valve 12 has an irregular or marred surface which will not seal properly with the O-ring.
The puller mechanism is then assembled by inserting puller 56 into bore 30 and thereafter threading collar 44 into threads 32 of core 28. Handle 54 is then threaded into the top end 56a of puller 56. Handle 54 is then pressed downwardly until fingers 58 spread slightly outwardly about stem 24 whereupon tangs 60 snap into groove 26. The person repairing then pulls upwardly on handle 54 until the upper edge 56a of puller 56 abuts the bottom surface of lip 47 of collar 44. The valve core 28 of the tool is then rotated to the position shown in FIG. 3 thereby isolating the pressurized system from the valve core 20 to be repaired.
Collar 44 is then unscrewed from core 28 and the puller 56 and core 20 withdrawn and the core 20 unsnapped to be either replaced or repaired as so desired.
To replace valve core 20, the process is reversed from that described above. For reinsertion, while the puller mechanism 56 may be utilized, it may be desirable to utilize a separate insertion tool (not shown). The insertion tool may be a tubular member having an outside diameter like that of puller 56 and having a smooth inner bore sized to slide over stem 24 and bear upon the top surface of plug 20. The use of such an insertion tool facilitates insertion as there is no need to utilize the tangs 60 since there is no need to hook and unhook the same. All the insertion tool need do is provide a means for pushing down on the plug 20.
It is desirable to reinsert valve core 20 in the position shown in FIG. 6, that is, so that zone control valve 12 is open. Such replacement will place the least pressure on core 20 which would tend to cause it to pop out. Once core 20 has been repaired and reinserted, it can have a tendency to be blown out of valve 12 by the pressure. This tendency is less pronounced during removal because the damaged seal tends to resist. This can be prevented by slightly loosening bolts 41 as shown in FIGS. 5 and 6 and inserting retainer flange 62 between the tool valve body 34 and around ears 14 of the zone control valve. After retainer plate 62 is inserted, the body 34 may be completely unbolted and the motor reattached and, once it has been substantially bolted down, retainer plate 62 may also be removed.
It is contemplated that various changes and modifications may be made to the zone control valve removal tool without departing from the spirit or scope of my invention as defined by the following claims. | A tool and method are disclosed for removing a valve core or element from a valve which is under pressure without requiring that the system be shut down and the pressure relieved. A tool having a passage therethrough sized to accommodate the valve element to be serviced is bolted over the valve and the valve element is drawn therein and the tool closed to isolate the passage and the element from the pressurized system thereby allowing the element to be repaired or replaced. | 1 |
BACKGROUND
Intravaginal devices such as diaphragms and other cervical barrier devices are useful for contraception and disease prevention. Such devices can also be used for collecting menstrual discharge, collection of vaginal samples, or to deliver therapies. A typical design of an intravaginal device consists of a flexible rim surrounding a hemispheric-shaped dome, often manufactured using a mold that simultaneously forms both the rim and the dome. The dome provides barrier, collection, and/or drug delivery functions, whereas the rim holds and supports the dome during insertion and during wear within the vagina.
Various designs and methods of construction are known. One of the most common designs includes a metal spring in the rim of the device to provide elastic force that restores the rim to its expanded configuration after being compressed during vaginal insertion. The spring is incorporated into the rim by a molding process that simultaneously creates the dome and covers the spring with a continuous and unbroken layer of elastomer. Other designs use rims that are entirely elastomeric without metal springs. Although molding the rim and dome as a single piece creates devices with smooth surfaces that provide comfort in use, the domes created by this method are relatively thick. This is because it is difficult to mold parts having a relatively large surface area as a thin piece. The dome portion must remain relatively thick to allow proper filling of the mold because the injected polymer must flow a long distance through a narrow mold cavity.
It is advantageous, however, for an intravaginal device to have a thin dome. Thin domes are compact when compressed for insertion, and they can be made very soft and compliant. To create a thin dome requires methods that employ assembly of the device from separate dome and rim pieces. The film piece is attached to the rim where it can be further shaped and expanded by thermoforming (softening by heating, and drawing by vacuum into a mold shaped to the desired final dome shape), which further reduces the dome thickness. In addition, the device assembled from separate pieces allows a single rim design to be used with multiple different dome shapes such as the roughly hemispheric shape of conventional diaphragms, or other dome shapes.
A significant disadvantage of diaphragms and similar devices assembled from a separate dome piece and a separate rim piece that has not been recognized or overcome in the prior art is the exposure of an unprotected and potentially harsh outer edge of the dome material upon attaching the dome to the rim. FIG. 1 , for example, illustrates a common rim design in the prior art having a circular cross-section with a width 18 less than or equal to its height 20 . As illustrated in FIG. 1 , the dome piece 10 is positioned for attachment at a typical attachment site 16 on the upper surface of the rim 12 . When attached, the dome piece edge 14 is disadvantageously exposed and unprotected.
A sharp edge may be created at an outer edge of a dome piece if the dome film is cut to shape before attachment. A rough or sharp edge just outside the attachment site can also be created with a known alternative assembly method of simultaneously attaching a plurality of domes to the top of a plurality of rims, employing a multi-headed welding tool. An oversized uncut piece of dome film is stretched over the multi-headed welding tool. The multi-headed welding tool presses through the sheet of dome film onto the rims, and the web of film outside the perimeter of the welding tool softens to form a weld line. The waste web is subsequently pulled free from the heat-softened weld line. Although precautions can be taken during manufacture to reduce roughness of the exposed edge, for example, by adding subsequent smoothing steps or shaping the welding tool to minimize residual roughness, these extra steps add cost and complexity, and may be only partially effective.
The outer edge of the attached film may be sufficiently rough or sharp to irritate or injure the vagina during insertion or wear, and irritate or injure the penis during sexual intercourse. Even if the weld-edge roughness is sufficiently minimal that detectable injury does not result, any roughness felt during insertion, wear or intercourse is disadvantageous.
Another disadvantage of attaching the dome to an unprotected surface of the rim is the resulting exposure of the edge of the dome to forces that may pull it loose from the rim. During insertion or with movement during wear, an exposed edge of the dome material may rub against epithelial surfaces, and, with sufficient purchase of the epithelium on the edge, may be pulled loose from the rim, especially if a local weakness in the attachment bond is present. Movement during intercourse may also contribute to detachment of the dome material due to traction on an exposed dome edge. Any detachment along the attachment bond or any separation of the dome material from the rim can compromise barrier function of the device. Even partial detachment that does not compromise the barrier function can create a crevice or flap between the dome and rim that is difficult to clean and reduces the suitability of the device to function as a re-usable device.
Also, diaphragms and similar devices may be difficult to grasp for positioning within or removal from the vagina. To remove a typical diaphragm, a user must grasp the device at the rim, generally by pushing the dome material up inside the perimeter of the rim to allow the fingertip to curve around the top of the rim from the inside, and then by pulling the rim downward and out of the vagina. Grasping the upper surface of the rim can be difficult since the dome material tends to interfere with access to this portion of the rim, and since the grasping finger must traverse the entire height of the rim to gain purchase on its upper surface.
SUMMARY
The present invention provides rim designs for diaphragms and similar intravaginal devices, which improve their manufacturability, ease of insertion, comfort in use, and ease of removal. These designs incorporate one or more recesses in the inner portion of a rim piece that provide a protected site on the rim for dome attachment, where a separate dome piece is positioned and attached. Attachment within a recess shields the potentially sharp or rough outer edge of the dome material from contact with epithelial surfaces, and improves comfort and safety. Incorporating one or more recesses into the inner portion of the rim also reduces the tendency of the rim to twist during compression, and thus improves its stability during handling before and during insertion. In certain embodiments of the invention, a thinned inner portion of the rim serves as a handle that can be easily grasped by a finger used to position the device and to remove the device from the vagina.
In an embodiment of the present invention, an intravaginal device is provided with a rim piece including an inner portion. The rim piece includes at least one recess associated with the inner portion of the rim piece. The device also includes a dome piece having a thickness. The depth of the recess is at least as great as the thickness of the dome piece. The dome piece is operably attached to the rim piece within a recess of the inner portion of the rim piece.
In an embodiment, a cross-sectional width of the rim piece of the device is greater than or equal to a cross-sectional height of the rim piece.
In an embodiment, a plurality of recesses are associated with the inner portion of the rim piece.
In an embodiment, the depth of at least one of the recesses is equal to the depth of at least one of the other recess.
In an embodiment, the depth of at least one recess is different than the depth of at least one other recess.
In an embodiment, the recesses associated with the inner portion of the rim piece define a thickness of the inner portion, wherein the thickness approaches the thickness of the dome piece.
In an embodiment, the dome piece is attached to the rim piece at a substantially central position between a top portion and a bottom portion of the rim piece.
In an embodiment, the dome piece is attached to the rim piece at a position away from a central position between a top portion and a bottom portion of the rim piece.
In an embodiment, the thickness of the inner portion of the rim piece is between about 1 and about 0.01 millimeters.
In an embodiment, the inner portion of the rim piece is adapted to function as a handle to position the device within a vagina and remove the device from the vagina.
In an embodiment, an outer portion of the rim piece includes at least one outwardly projecting circumferential bead.
In an embodiment, an outer portion of the rim piece includes at least one circumferential groove.
In an embodiment, the dome piece is attached to the rim piece by an attachment method selected from the group consisting of: thermowelding, ultrasonic welding, radiofrequency welding, solvent welding, and adhesive attachment.
In an embodiment, a method of forming an elastomeric dome piece of the intravaginal device of the claimed invention is provided. The method includes, after attaching said dome piece to said rim piece, softening the dome piece by heating and drawing the dome piece by vacuum into a mold. The mold is shaped to a desired dome piece shape.
In another embodiment, a method of producing and attaching an elastomeric dome of an intravaginal device to a rim of the device is provided. The method includes forming a rim having an inner portion. The inner portion includes at least one recess. The method also includes placing the rim over a mandrel so that the inner portion of the rim contacts the mandrel. The method further includes applying a polymer and solvent mixture to the rim and mandrel. The method further includes allowing the mixture to coat the mandrel such that the mixture contacts the inner portion of the rim. The method further includes allowing the solvent to evaporate.
In an embodiment, the method of applying the polymer and solvent mixture to the rim and mandrel includes spraying the polymer and solvent mixture to the rim and mandrel.
In a further embodiment, a method of removing substances from the vagina is provided. The method includes operably positioning in the vagina of an individual in need thereof an intravaginal device. The device includes a rim piece including an inner portion and an outer portion and a dome piece having a thickness. The rim piece includes at least one recess associated with the inner portion. The recess includes a depth wherein the depth of the recess is at least as great as the thickness of the flexible dome piece. The dome piece is operably attached to the rim piece within the recess of the inner portion of the rim piece. The method also includes removing the intravaginal device from the vagina.
In an embodiment, the rim piece includes at least two recesses. The recesses oppose one another to define a dome attachment site at a substantially central position along the inner portion of the rim piece.
In yet another embodiment, a method of preparing an intravaginal device is provided. The method includes providing a rim piece including an inner portion. The rim piece includes at least a first recess and a second recess associated with the inner portion. The method also includes placing the rim piece on a rim support. The rim support is positioned within the first recess of the rim piece. The method further includes positioning a dome piece within the second recess of the rim piece and attaching the dome piece to the inner portion of the rim piece.
In yet a further embodiment, a method of preparing an intravaginal device is provided. The method includes placing dome material on a holding surface and providing vacuum pressure from the holding surface that is sufficient to maintain the dome material in a position on the holding surface. The method also includes cutting the dome material to form a dome piece. The method further includes providing a rim piece including an inner portion. The rim piece includes at least a first recess and a second recess associated with the inner portion. The method additionally includes placing the rim piece on a rim support. The rim support is positioned within the first recess of the rim piece. The method includes positioning the dome piece on the holding surface within the second recess of the rim piece and attaching the dome piece to the inner portion of the rim piece.
In an embodiment, the method includes transferring the dome piece from the holding surface to the rim piece. Transferring the dome piece includes at least reducing vacuum pressure from the holding surface.
In an embodiment, the method includes transferring the dome piece from the holding surface to the rim piece. Transferring the dome piece includes providing vacuum pressure from the rim support sufficient to substantially hold the dome piece within the second recess of the rim piece.
In an embodiment, the method includes providing vacuum pressure from the rim support sufficient to maintain the rim piece in a position on said rim support.
It is an advantage of the present invention to provide a device with an improved rim design.
Another advantage of the present invention is to provide a protected attachment site for the edge of the dome piece.
Yet another advantage of the present invention is to provide a device with a rim having a dome attachment site located substantially symmetrically between the top and bottom edge of the rim.
A further advantage of the present invention is to provide a device that is easier to remove.
An additional advantage of the present invention is to provide a device with a rim shape that aids in the retention of beneficial agents during insertion.
Yet another advantage of the present invention is to provide a device that can collect and remove materials from the vagina.
Yet an additional advantage of the present invention is to provide a device that more effectively cleanses the vagina of secretions and prior doses of medication, thus preventing accumulation and subsequent vaginal discharge.
Yet a further advantage of the present invention is to provide a method for producing intravaginal devices.
Yet another advantage of the present invention is to provide a device that is less prone to twisting when compressed for insertion.
Additional features and advantages of the present invention are described in, and will be apparent from, the following Detailed Description and the figures.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a cross-section of a portion of a rim and dome piece of an intravaginal device, with the dome piece positioned above the rim in preparation for attachment at a site on the rim where the dome piece is conventionally attached.
FIG. 2 is a cross-section of a portion of a rim and dome piece of an intravaginal device, with the dome piece positioned above the rim in preparation for attachment within a recess in the rim of one embodiment of the present invention.
FIG. 3 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 4 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 5 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 6 is a top down view of a rim of one embodiment of the present invention that is divided into segments demarcated by radial dashed lines with different cross-sectional profiles that are shown in insets A and B.
FIG. 7 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 8 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 9 is a cross-section of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 10 is a cross-sectional view of a portion of a rim and dome piece of an intravaginal device illustrating attachment of the dome piece within a recess in the rim of one embodiment of the present invention.
FIG. 11A is a cross-sectional perspective exploded view of the intravaginal device of one embodiment of the present invention with an attached and formed dome.
FIG. 11B is a cross-sectional view of an intravaginal device of one embodiment of the present invention with an attached and formed dome.
FIG. 12A is a cross-sectional perspective view of an intravaginal device of one embodiment of the present invention with an attached and formed dome.
FIG. 12B is a cross-sectional view of an intravaginal device of one embodiment of the present invention with an attached and formed dome.
FIG. 13A is a perspective view of a portion of an apparatus used to manufacture dome pieces according to the method of one embodiment of the present invention.
FIG. 13B is a cross-sectional perspective view of a single operational component of an apparatus used to attach a dome piece to a rim piece according to the method of one embodiment of the present invention.
DETAILED DESCRIPTION
The present invention relates to intravaginal devices. In particular, the present invention relates to an intravaginal device including a rim piece and a dome piece. The rim includes at least one recess on its inner surface into which the outer edge of the dome piece is placed and attached. Positioning the edge of the dome piece in this recess prevents the potentially sharp or rough outer edge of the dome piece from contacting either the vaginal or penile epithelium and protects the edge of the dome from being peeled away from the rim as may occur if the dome piece was attached on an exposed surface of the rim. As discussed above, FIG. 1 illustrates a typical design of the prior art where a dome piece edge 14 is disadvantageously exposed when attached on the upper surface of a rim 12 with a circular cross-section having a width 18 equal to its height 20 .
Referring now to the remaining drawings, as illustrated in FIG. 2 , the intravaginal device of one embodiment of the present invention includes a rim 12 having a substantially round cross-section. The rim 12 may include a recess associated with an inner aspect of the rim. The recess may be located along any portion of the inner aspect of the rim including a peripheral aspect of the rim as illustrated in FIG. 2 . The recess may include a depth 22 and a width 24 . The recess width 24 (measured in the horizontal dimension) may be at least sufficient to define an attachment site 16 adapted to receive the outer edge 14 of a dome piece 10 . The recess depth 22 (measured in the vertical dimension) may be at least as great as the thickness of the dome piece 10 , to effectively shield the edge 14 from contact once attached within the recess.
In one embodiment, the depth 22 of the recess into which the dome piece 10 is positioned and attached is substantially greater than the thickness of the dome piece. Among other advantages, this feature has the advantage of partially shielding the dome attachment site from the full extent of heating it would otherwise experience during subsequent shaping of the dome piece by thermoforming (see below). This shielding is due to the location of the attachment site 16 in the recess, which, if sufficiently deep, creates a shadowing or protective effect, reducing the heating received from a wide thermal source that may be used to soften the dome piece in preparation for shaping. When using a wide heat source as is used in manufacturing where multiple devices are thermoformed at the same time, only the portion of the heat source directly above a recessed dome will radiate heat to the edge of the recess, the location of the attachment site. Reducing additional heating to the attachment site 16 after the attachment step is advantageous, since cumulative “heat-history” can reduce polymer resilience, can induce undesirable yellowing, and can reduce the strength and integrity of the bond between dome piece 10 and rim piece 12 .
The recess width 24 is preferably sufficient to provide a secure and reliable attachment site 16 for the dome piece 10 to the rim 12 . In one embodiment, at least one recess defines a substantially horizontal surface associated with the inner portion of the rim. The width of the recess 24 (measured in the horizontal dimension) is advantageously between about 1 and about 5 mm, more preferably between about 2 and about 4 mm in width.
A substantial recess width 24 associated with the rim is also beneficial in holding certain preferred dome designs in place during compression for insertion. For example, the sombrero-shaped dome described in U.S. Pat. No. 6,474,338 may be used with any of the rim designs of the present invention including, as illustrated in FIG. 12 , the rim design illustrated in FIG. 5 . The upwardly projecting central portion of the sombrero-shaped dome, together with any added beneficial agent, is pulled down by gravity as the device is held in preparation for the insertion step. The dome and/or any applied beneficial agent can fall through the plane of the rim defeating the proper function of this dome design. A generous width of the recess of the rim helps prevent this by extending across the gap between opposing sections of the compressed or partially compressed rim.
Non-circular cross-section rim designs are used in existing intravaginal devices to reduce the bowing and twisting associated with circular cross-section rim designs during compression of the device in preparation for insertion. Formation of an awkward shape such as a “twisted figure-8” configuration complicates proper insertion of the intravaginal device. Metal-free, fully elastomeric rims with round cross-sections are even more prone to bowing and twisting.
In one embodiment, the cross-sectional width of the rim 18 is greater than or equal to the cross-sectional height 20 of the rim. FIG. 3 , for example, illustrates another embodiment of the rim 12 of the present invention having a substantially non-circular cross-section. The embodiment illustrated in FIG. 3 includes a rim having a cross-sectional width 18 greater than or equal to a cross-sectional height 20 of the rim forming in this case a substantially square cross-section rim. Similar to the embodiment illustrated in FIG. 2 , the embodiment illustrated in FIG. 3 includes a recess in the upper surface of its inner portion defining an attachment site 16 adapted to receive the outer edge 14 of a dome piece 10 .
The rim must have substantial width in order to provide a sufficiently ample attachment site along the inner portion of the rim for assembly of the dome piece to the rim piece while retaining sufficient strength and resiliency in the outer portion of the rim to create an adequate outward holding force to hold the rim in proper position in the vagina. In one embodiment, the width of the rim is advantageously made less than about 10 mm, and more advantageously between about 5 and about 8 mm. In one embodiment, the upper, non-recessed outer portion of the rim is sufficient to retract epithelial surfaces away from the potentially rough edge 14 of the dome material 10 . An ample total rim width is also advantageous to provide a wide enough inner portion to be easily grasped by the retrieving finger. The described range of widths is also advantageous in order to avoid the thinned inner portion of the rim being excessively wide and thereby being prone to press against the cervix, which will lie within the perimeter of the rim.
At the same time, there are practical upper limits on rim height 20 . If the rim height is excessive, it may extend downward from behind the pubic bone during wear, and be obstructive during intercourse. To this end, the height of the rim is advantageously made less than about 10 mm, and more advantageously, between about 5 and about 8 mm. Thus, the need for a substantial rim width 18 , and the limits on the rim height 20 , make it advantageous for the rim width 18 to be greater than or equal to the rim height 20 .
In one embodiment, the dome piece is attached to at least the substantially horizontal surface of an inner recessed portion of the rim. The dome piece may also be attached to at least a substantially vertical and a substantially horizontal surface of the inner recessed portion of the rim.
In another embodiment, illustrated in FIG. 4 , a rim 12 includes more than one recess associated with the inner portion of a rim. In one embodiment, the rim includes multiple recesses. A recess may be associated with a top portion 13 of the rim and a recess may be associated with a bottom portion 15 of the rim. The recesses may have substantially equivalent dimensions and/or be positioned symmetrically along the inner portion of the rim on either side of an approximate vertical center 25 of the rim. It should be appreciated that symmetry in design is advantageous during manufacture and use of intravaginal devices. For example, a symmetrical rim design may not require an “up-down” orientation step during manufacture of the rim. Avoiding an orientation step is a significant advantage during high-volume manufacturing.
An additional benefit of providing one or more recesses in the inner portion of the rim is a reduction in the tendency of the rim to twist awkwardly when compressed for insertion.
In an embodiment illustrated in FIG. 5 , not only the rim, but also the entire device may be made essentially symmetrical in regard to its up-down orientation. In the embodiment illustrated in FIG. 5 the cross-section of the rim of the intravaginal device is substantially symmetrical above and below an approximate center 25 of the rim. In such an embodiment, the symmetrical recesses associated with the top portion 13 and bottom portion 15 of the rim are made sufficiently deep to locate the attachment site 16 to the inner portion of the rim at the approximate center 25 of the rim. In an embodiment having a compliant dome attached to the substantially central portion 25 of the inside of the rim, the dome can be deployed in either direction and, therefore, the device can be inserted without regard to up-down orientation. Thus, in the embodiment shown in FIG. 5 , the device can be placed in the vagina with either surface pointing upward without the user having to manipulate the device into a correct “up-down” orientation.
As compared to the embodiments illustrated in FIGS. 2 , 3 and 4 , FIG. 5 further illustrates that, in an embodiment, the dimensions of the recess of the inner portion of the rim can vary. In the embodiment illustrated in FIG. 5 , the recesses are sufficient to form a rim that is significantly more compliant along its inner portion than the rest of the rim. The dimensions of the recesses can be manipulated to form a rim that is not too thick along its inner portion, thus preventing the rim from having a stiff and sharp edge that can press against the cervix. In addition, the dimensions of the recesses may be manipulated to form a rim that is sufficiently thick along its inner portion to provide a strong and robust attachment site. Additionally, a portion of the rim that is too thin will also not be stiff enough to serve as a suitable handle (see below). Optimizing the compliance of the rim along its inner portion offers sufficient stiffness for the inner portion of the rim to be easily grasped and to function as a handle (see below) while being sufficiently compliant to prevent its inward facing edge from being a sharp and potentially damaging contact point with the cervix. Moreover, if the rim has an excessively thin portion, it may be difficult during fabrication of the rim to fill this portion in a mold or during extrusion molding through a die. To achieve appropriate softness or compliance in one embodiment, opposing recesses in the inner portion of the rim may advantageously define a rim having an inner portion thickness 26 of between about 1 and about 0.01 mm in the vertical dimension, and, more advantageously, between about 0.5 and about 0.1 mm in thickness. Thus the thickness of the inner portion can, in one embodiment, advantageously approach the thickness of the dome material (see below).
Being an intrinsic part of the rim, the inner portion of the rim may possess a stiffness-discontinuity with the dome material by virtue of the greater stiffness of the rim material. This stiffness-discontinuity at the junction of the dome and rim may allow this junction to serve as a handle. To this end, a further advantage of the design illustrated in FIG. 5 is that the inner portion of the rim can function as a handle that provides a significantly more favorable gripping site for the user to position and to remove the device. In such an embodiment, the inner portion of the rim is more easily grasped than the rims of prior designs. For example, to remove a device having a rim with a prior design, the user must direct a retrieving finger to generally reach inside the rim, all the way to the upper edge of the rim while pushing the dome out of the way to access the edge of the rim. Access to this area may be difficult with conventional diaphragms and similar intravaginal devices since their relatively thick and non-compliant domes can interfere with grasping the rim. In contrast, the thin dome material characteristic of some embodiments of the present invention can be less interfering, and the recessed inner portion of the rim designs of the present invention may enable the retrieving finger of the user to reach the inner portion of the rim at a point substantially below the upper edge of the rim with less need to move the dome material out of the way as is required with conventional diaphragms.
An additional advantage of the embodiments illustrated in FIGS. 5-11 having a substantially central attachment site, and hence takeoff point, of the dome includes an improved efficiency in collecting and removing secretions from the vagina and/or substances that have been applied to the vagina. To this end, in one embodiment, the devices of the present invention may be used as a vaginal cleansing system. This improved efficiency of removal of substances from the vagina is due, in part, to the substantially central, or minimally asymmetric ( FIG. 7 ) attachment site, and, hence, takeoff point of the dome. In one embodiment, the configuration of the rim formed by opposing recesses associated with the inner portion of the rim can give the rim cross-section a substantial “T” shape that has been laid on its side, with the inner portion of the rim being the stem, and the outer portion of the rim being the arms of the “T”. The arms of the “T” can serve the function of gentle scrapers or “squeegees”, that, as the device is withdrawn from the vagina, cleanse the vaginal epithelium of adherent secretions, menstrual fluid, or applied substance on one or both sides of the device. As the device is pulled over the epithelium, the arms formed by the rim design of the present invention can efficiently wipe fluids off the vaginal walls, collect them within the perimeter of the rim, and substantially remove them from the vagina along with the device. Such an effective two-sided squeegee action may reduce the amount of discharge from the vagina after intercourse, or after application of medications.
Devices of the described embodiments thus can be used as a vaginal cleansing system, allowing effective cleansing without the multiple negative health outcomes associated with vaginal douching (Martino et al, 2004). More effective vaginal cleansing can be useful during or after menses, after sexual intercourse, or in the presence of vaginal discharge diseases. Prior designs of intravaginal devices, wherein the dome film is attached to an exposed edge of the rim, are disadvantageous in that an effective squeegee function may only be achieved, if at all, on the surface opposite the dome attachment. The surface with the dome attachment site will not effectively collect substances from the vaginal wall upon withdrawal of the device because the dome will prevent material from being gathered within the perimeter of the rim.
The rim design illustrated in FIG. 5 and other embodiments where the inner portion of the rim is substantially thinned is also far less susceptible to twisting or bowing upon compression of the device for insertion than round or even substantially square rim cross-sections. However, even the embodiments of rims having substantially thinned inner portions similar to the embodiment illustrated in FIG. 4 still have some tendency to twist. Accordingly, one embodiment includes a packaging system that holds the device in an oval shape until the device is removed from the package. Packaging the device in such a way results in substantial further reduction in the tendency of the device to twist when compressed for insertion.
It will be appreciated that, to serve particular purposes, additional embodiments within the scope of the present invention may incorporate combinations of different cross-sectional rim profiles in different segments along the perimeter of the rim. For example, in one embodiment, the rim includes one or more rim segments with an outer rim portion shaped to a substantially round cross-section, while retaining the configuration of the inner portion of the rim to provide an attachment site and protect the edge of the dome. This segment or segments can be placed at sites where the device may be particularly prone to contact the penis during intercourse, thus beneficially maximizing the radius of curvature of potential contact points between the rim and penis, and thereby improving comfort. Portions of the rim of the intravaginal device most likely to contact the penis are those portions of the rim that lie along the midline of the vagina during wear, and, in particular, the portion of the rim closest to the vaginal introitus. Thus, one such rounded segment can be provided where it can be positioned substantially behind the pubic bone.
Alternatively at least two rounded segments can be provided. The embodiment illustrated in FIG. 6 includes a rim divided into four segments having different cross-sectional profiles. As illustrated in inset A, the lateral segments 27 a and 27 b include an outer portion of the rim characterized by a profile substantially similar to the profile illustrated in FIG. 5 . As illustrated in inset B, the midline segments 28 a and 28 b include an outer portion of the rim characterized by a substantially rounded cross-sectional profile. The rim profile may include a recessed inner portion as previously described for other embodiments. In use, at least one of the midline rim segments 28 a can be positioned substantially behind the pubic bone, and the other segment 28 b substantially within the posterior fornix.
Other embodiments can include modified segments of the rim cross-sectional shape with reduced rim cross-sectional dimensions at one or more sites. In one embodiment, the rounded outer portion of the rim may include a smaller cross-sectional dimension. This creates two hinge-like portions along the rim due to an increased flexibility associated with reduced cross-sectional portions along the rim dimension of these segments. These flexible segments can aid in folding the device during compression for insertion.
In one embodiment a midline segment may be tipped upward slightly out of the plane of the rest of the rim. This upwardly angled midline segment can be positioned substantially behind the pubic bone during wear. The upward tilt advantageously can aid in positioning that portion of the device further behind the pubic bone, and can separate it further from contact with the penis during intercourse. Other variations in the cross-sectional shape of the rim or of one or more segments of the rim can be envisioned within the scope of the present invention, so long as the rim segments incorporate the recessed inner rim portion in such a fashion as to create a protected attachment site for a separate dome piece.
FIG. 7 illustrates another embodiment of the present invention including opposing recesses associated with the inner portion of the rim. The recesses can be positioned opposite one another in an asymmetrical fashion along the inner portion of the rim to define a dome attachment site at a position away from a substantially vertical center 25 of the rim. To this end, the vertical extent or depth of the recesses in the inner portion of the rim may be different with one recess 22 being deeper than the other recess 23 , resulting in the attachment site along the inner portion of the rim being located asymmetrically at a position away from a central position 25 between a top portion 13 of the rim and a bottom portion 15 of the rim.
Although equivalently dimensioned and symmetrically positioned recesses of the inner portion of the rim are advantageous in avoiding the need for orientation steps in manufacture and insertion as described above, there are also advantages for embodiments with asymmetrical recesses of the inner portion of the rim. For example, different dimensions and asymmetric positioning of the recesses of the inner portion of the rim may change the degree to which the device bows when compressed. It should be appreciated that slight downward bowing can be advantageous since this folded configuration can help the leading edge of the rim pass easily below the cervix when the device is being inserted into the vagina. Moreover, asymmetrical recesses can form an inner rim portion of the rim that is oriented toward the bottom of the rim and, thereby, further improve access to the inner portion of the rim during retrieval from the vagina.
Other features of the rim design of the present invention may include providing a more secure gripping surface on the outer surface of the rim. For example, in one embodiment, the outer rim surface is shaped to provide at least one outward projecting bead 29 , as illustrated in FIG. 8 , or, in another embodiment, at least one groove 30 , as illustrated in FIG. 9 . Other features to enhance the grip on the outer rim surface may include, but are not limited to, multiple beads and/or grooves, cross-hatching, or any other suitably shaped or textured surface which provides a more secure grip when the rim is held between the fingers for compression and insertion and/or contributes to maintaining the position of the device in the vagina. It should be appreciated that a secure grip is advantageous, since intravaginal devices are often used with lubricating gels or creams that may contain at least one active ingredient or any other beneficial agent such as spermicides, antivirals, antibacterials, antifungals, vaccines, hormones etc. The lubricating nature of these gels or creams makes the rim slippery; thus, a gripping feature is particularly beneficial.
It should be appreciated that other shapes or conformations of recesses can be associated with the inner portion of the rim to form a suitable attachment site for the dome piece and to achieve additional benefits. For example, the shape of the recesses that define the shape of the inner portion of the rim can be rounded or curved. In one embodiment illustrated in FIG. 10 , a recess can form an inner portion of the rim that is tapered through to a substantially horizontal inner portion of the rim. The shape of the recesses may define an inner portion of the rim that approaches the thickness and compliance of the dome piece material. Advantages of this tapered shape include maintaining the strength of the inner portion of rim while producing a substantially thin and, therefore, soft or flexible inward-facing edge in order to avoid any harsh impingement on the cervix which will be located within the perimeter of the rim during wear within the vagina.
The rims of the present invention can be made by injection molding of thermoplastics. Molding of polymers such as silicone into the rim profiles of the present invention can be used wherein the polymerization and/or cross-linking occurs in situ within the mold. Alternatively, the rim profile can be formed by extrusion from a die and cut to length. The two ends of the rim may be joined to form a closed, substantially circular or substantially oval shape, and fused by any suitable means such as thermowelding, ultrasonic welding, radiofrequency welding, use of a suitable adhesive or any other suitable method of securing together the ends of the rim.
Materials suitable for fabrication of intravaginal devices of the present invention include, without limitation, various thermoplastic polyurethanes, ethylene vinyl acetate, polyethylene, styrene-butadiene-styrene, styrene-ethylene/butylene-styrene, and silicone. Mixtures of two or more of these materials may also be employed. Different materials, or different hardness grades of the same materials can be used for the separate dome and rim pieces. For example, if the attachment method includes a step to heat and soften the dome and rim surfaces to be bonded, it is advantageous that dome and rim be made of the same material. If the materials of the dome and rim are not the same, each may contain at least some percentage of a material present in the other component in order to enhance the success of bonding by a heating method. It is generally advantageous for the dome material to be chosen for softness and drape, and for the rim material to be chosen for greater stiffness to provide an adequate outward holding force.
The rim designs of the present invention can be combined with dome pieces of any suitable shape or configuration. For example, a simple, substantially hemispheric shape of conventional diaphragms can be combined with the rim designs of the present invention as illustrated in FIGS. 11A and 11B . Other dome shapes can be combined with the rim designs of the present invention including, in one embodiment, the sombrero-shaped dome discussed above and illustrated in FIGS. 12A and 12B . In one embodiment, the dome film is shaped to its desired shape by vacuum thermoforming or other methods known in the art once the dome piece is attached to the dome attachment site 16 of the rim. In another embodiment, the dome film is shaped prior to being attached to the dome attachment site 16 of the rim. Moreover, if shaped prior to being attached, the dome film can be shaped by any suitable method and not restricted to thermoforming from a flat sheet of film.
Referring to FIGS. 13A and B, an embodiment of the present invention includes an alternative method of cutting, positioning, holding in place, and attaching a plurality of rims and dome pieces that is suitable for high-volume manufacturing. The method includes placing a sheet of dome material film 12 a on a holding surface of each of an array of holding pedestals 30 . The holding surfaces of the holding pedestals may be sized to the dimensions necessary for subsequent formation of the dome piece 12 of the intravaginal device. The dome material film 12 a can be reversibly held or affixed to the holding surface of each of the holding pedestals 30 by applying vacuum to the film through a plurality of channels 32 emerging through the holding surface of the holding pedestals 30 .
The method can further include providing a matching set of at least partially hollow cutting cylinders 34 . Each of the cutting cylinders 34 may be positioned opposite one of the holding pedestals 30 and each of the cutting cylinders 34 may include inside dimensions substantially equal and corresponding to outside dimensions of the holding surface of the holding pedestal 30 . The cutting cylinders 34 can be pressed down over the film 12 a beyond the holding surfaces of the holding pedestals 30 into a bypass cutting position. Accordingly, the cutting cylinders 34 can function as bypass cutters, trimming the film into a set of disc-shaped dome pieces 12 having a diameter substantially equal to the diameter of the holding surface of the holding pedestal. In one embodiment, heat can be applied to the cutting cylinders 34 to enhance the cutting action achieved. After retracting or removing the cutting cylinders from the bypass cutting position, the web of film 12 a from which the dome pieces 12 have been cut is removed. It will be appreciated that the orientation of the holding pedestals and cutting cylinders described above can be altered as needed for efficient manufacture.
As illustrated in FIG. 13B , in one embodiment, the rim 10 to which a dome piece 12 is to be attached can be placed on a rim support pedestal 36 . Each rim support pedestal 36 may be adapted to support the inner portion of a rim 10 to which a dome piece 12 is to be attached. In an embodiment, a plurality of rim support pedestals 36 are provided. These rim support pedestals 36 can be arranged in an array configured to match an array of holding pedestals 30 such that each holding pedestal is positioned opposite one of the rim support pedestals. In one embodiment, each of the rim support pedestals 36 is supplied with channels 32 on at least a perimeter of a support surface through which vacuum can be applied to hold the rim piece 10 in place. In one embodiment, each of the rim support pedestals 36 is supplied with channels 32 in a substantially central portion of its support surface through which vacuum can be applied to hold the dome piece 12 in place when positioned for attachment to the rim piece 10 . The array of holding pedestals 30 and their vacuum-held dome pieces 12 may be inverted, and operably positioned to insert each of the plurality of dome pieces 12 into a recess of each of the plurality of rim pieces 10 operably positioned on the rim support pedestal 38 to receive the dome piece 12 . Vacuum may be applied to the central portion of the support surface of the rim support pedestals 38 to hold the dome piece in a precise position against the inner portion of the rim 10 for attachment to the rim. Upon suitable positioning of the dome piece within the recess of the rim, vacuum from the holding pedestals 30 may be discontinued, and the holding pedestals 30 removed or retracted to a retracted position leaving each of the dome pieces 12 in a position to be attached to the rim pieces 10 supported by the rim support pedestals 36 .
In an embodiment of the present invention the subsequent dome attachment step is by thermowelding with an array of weld tools distinct from the array of holding pedestals. In another embodiment, welding tools are incorporated into the holding pedestals by providing a heating element along the perimeter of their holding surfaces.
The dome film can be manufactured by any suitable means. In an embodiment including a dome piece comprising a flat film attached to a rim of the present invention with subsequent steps to form the dome, the film can be manufactured by calendaring, blow molding or extrusion. The dome material can be any desired thickness, although, as described above, it is advantageous that the completed dome be relatively thin, preferably less than about 1 mm, and more preferably less than about 0.2 mm in thickness. To retain adequate strength, and to reduce the chance that holes will be created during manufacture, it is generally preferable that the dome have a minimal thickness of about 0.05 mm.
Other methods for creating and attaching a dome to the rims of FIGS. 5-12 include a polymer/solvent dipping or spraying method. The dipping method includes attaching the rim to a mandrel. The mandrel is dipped in a polymer/solvent mixture so that the mixture coats the mandrel and contacts the inner portion of the rim. The solvent is subsequently removed by evaporation.
In polymer/solvent-based methods, the thin inner portion of the above-described rims can be useful to provide an efficient seal to the mandrel. An effective seal to the mandrel is preferable to prevent the polymer/solvent mixture from moving higher on the mandrel than is desirable, and from being deposited at sites other than those intended. The rims of the present invention, such as those described in FIGS. 5-12 , are well suited for this process, since the thicknesses of the inner portions of the rims described in FIGS. 5-12 can be made sufficiently thin to make these inner portions compliant and flexible. To achieve sufficient compliance to produce an effective seal to the mandrel, it is advantageous that the thickness of the inner portion is between about 1 and about 0.01 mm, and more advantageously between about 0.5 and about 0.1 mm. It should be appreciated that the thickness of the inner portion of the rim necessary to achieve sufficient compliance may vary from these disclosed measurements, depending on the material(s) of the rim. As discussed above, the greater stiffness of the inner portion of the rim in comparison to the attached dome enables the inner portion of the rim to serve as a handle that assists positioning in the vagina and removal from the vagina, just as with a dome film attached by thermowelding or other means of attaching a preformed dome film.
An additional benefit of rim designs of the present invention includes a more favorable compatibility with common polymer/solvent methods of dome fabrication: the inner portion of the rim can be positioned to selectively or exclusively contact the solvent/polymer mixture without contacting the outer portion of the rim. To this end, the mandrel may deflect the free edge of the inner portion of the rim to allow the inner portion of the rim to project downward, beyond the lower edge of the outer portion of the rim and toward a solvent/polymer bath or a spray-head. To further position the rim in an advantageous position for attachment of the dome piece, the lower aspect of the outer portion of the rim can be twisted upward and outward.
Certain embodiments of the present invention are helpful to further enable exclusive contact of the inner portion of the rim with the solvent/polymer mixture. One embodiment arranges the recesses in the rim to position the dome attachment site on the inner portion of the rim in closer proximity to a peripheral edge of the rim as it is held for dipping. This allows the dome attachment site to be optimally positioned to enable sufficient downward deflection upon contact with the mandrel. In addition, the recesses in the rim may define a width of the inner portion of the rim that enables sufficient downward deflection upon contact with the mandrel. Such a width can be advantageously made between about 2 and about 6 mm, and more advantageously between about 3 and about 4 mm.
Dipping methods to create thin films of latex, polyurethane, or other polymers, may also be employed to create the dome. For example, solvents that are useful for polyurethane dip molding include tetrahydrofuran, dimethyl acetamide N-methylpyrrolidone, and dimethyl formamide. Additional agents can be added such as weak solvents or non-solvents of polyurethane to adjust viscosity and enhance removal of solvents after dipping. These agents include aliphatic alcohols, aliphatic amines, aliphatic and aromatic hydrocarbons. Polymeric concentrations in the polymer/solvent mixture can be advantageously from about 5 to about 10% by weight, and the viscosity of the polymer/solvent mixture can be advantageously controlled between about 500 and about 1000 cP.
The mandrel and attached rim can be slowly lowered into the dip solution, allowed to remain there for a few seconds, and slowly removed. The solvents can be allowed to evaporate. The mandrel can be rotated to control the thickness of various portions of the dome through gravity-induced movement of the dip solution before its solvent evaporates. Heat, vacuum, and solvent recovery steps may be included in the solvent evaporation process to speed drying, and to reduce material costs and environmental pollution. Other suitable methods for the dip molding of latex films and other polymer films are known in the art, and can be chosen to fabricate domes by polymer/solvent dipping with appropriate adjustments of polymer concentration, solvents, and evaporation conditions.
Alternatively, the polymer/solvent mixture can be sprayed onto the rim and mandrel assembly.
An advantage of attaching the solvent-dipped or sprayed dome to the inner portions of the rims of the present invention, includes the removal of solvent from the rim during the solvent evaporation stage than if the solvent had contacted and penetrated into a thicker portion of the rim.
EXAMPLE 1
A rim with a generally round cross-section, as illustrated in FIG. 1 , is fabricated from aromatic polyurethane by injection molding. Thermoplastic polyurethane film of 0.0075-inch (0.19 mm) thickness is welded to the top surface of the rim using a heated welding tool. During the application of heat and pressure, the excess film is pulled upward and away from the weld line, parting the film at the melted edge of the weld line. The attached flat film is then heated with hot air, and vacuum thermoformed into the desired dome shape. The outer edge of the weld line is found to be rough to the touch. This roughness is fully exposed, accessible, and easily felt.
When the rim is compressed between the thumb and fingers, as in preparation for insertion, the rim contorts into undesirable configurations. First, as seen from the side view, it bows dramatically into a pronounced “C” shape. In addition, as seen from above, it twists into a twisted “figure-8”. Either of these configurations makes it difficult to hold and to maintain control of the compressed rim, making insertion into the vagina more difficult. Both of these inconvenient contortions are also commonly observed with traditional contraceptive diaphragms.
A variant of the round rim is molded with flat inner surfaces at the point of compression, allowing more stable mating of the inner rim surfaces as they are pressed together. This configuration does not significantly improve the bow and twist problems described above. An additional variant with a tongue and groove interlock feature machined into the flat region on the inside of the rim is fabricated, but, again, this does not significantly reduce the bowing or twisting.
EXAMPLE 2
A rim 12 with a cross-sectional configuration as shown in FIG. 8 that includes an outward facing bead on the outer surface of the rim is molded of thermoplastic polyurethane. This design is an example of the general strategy illustrated in FIG. 5 , wherein the inner portion of the rim is sufficiently recessed such that the inner portion of the rim forms an attachment site for the film, is positioned substantially at the vertical center between a top portion and a bottom portion of the rim to make the rim essentially symmetrical for simplicity in manufacture and for convenience during insertion. A dome piece made from a pre-cut disk of 0.0075-inch (0.19 mm) thick polyurethane film is laid over the inner portion of the rim and attached by thermowelding. The flat film is shaped into a dome configuration ( FIG. 11 ) using vacuum thermoforming, resulting in a final dome film thickness of 0.002 to 0.005 inch (0.05 mm to 0.13 mm).
The outer edge of the film is found to be highly and advantageously inaccessible and protected due to its location within the deep recess in the rim. The non-recessed outer portion of the rim prevents contact with any roughness of the cut edge of the dome film. The tendency of the rim to bow or twist upon compression is greatly reduced in comparison to the device of Example 1. The bead on the external surface of the rim provides good security in holding the rim for compression and insertion. The rim is symmetrical and can be positioned with either side up during the dome attachment step of manufacture. Similarly, the completed device is essentially symmetrical, particularly where the dome is formed as in FIG. 11 as a compliant hemispheric shape. The completed device can be inserted with either side up, making insertion more convenient. Finally, the inner portion of the rim can be securely engaged by the index finger for removal from the vagina.
EXAMPLE 3
A rim as shown in FIG. 9 is molded of thermoplastic polyurethane. The design is again similar to that illustrated in FIG. 5 , with the inner portion of the rim being deeply recessed symmetrically at its top and bottom. The outer surface of the rim contains a groove as a grip feature rather than the bead of Example 2. A dome piece made from a pre-cut disk of polyurethane film is welded to the inner portion of the rim (at the floor of the recess) by thermowelding. The attached flat film is then shaped into a dome configuration ( FIG. 12 ) using vacuum thermoforming.
As in Example 2, the edge of the film attached to the rim of Example 3 is advantageously protected, due to its location deep within the recess and away from the external surface of the rim. The higher vertical profile of the outer portion of the rim prevents contact with any roughness of the cut edge of the dome film. The finished device demonstrates much less tendency to twist or bow compared to the device in Example 1. The outward facing groove provides for secure gripping of the device while compressing it for insertion. Lastly, the inner portion of the rim is easily engaged by the index finger as for positioning within or removal from the vagina.
It will be understood that although this and the previous examples employ fully elastomeric rims, rims that incorporate metal springs are also within the scope of the present invention. Likewise, intravaginal devices with rims providing the improved dome attachment features described in the present invention can also serve additional or alternative functions such as the delivery of beneficial agents, and collection and removal of substances from the vagina.
It should be understood that various changes and modifications to the presently preferred embodiments described herein will be apparent to those skilled in the art. Such changes and modifications can be made without departing from the spirit and scope of the present invention and without diminishing its intended advantages. It is therefore intended that such changes and modifications be covered by the appended claims. | The present invention provides improved rim designs for diaphragms or any similar intravaginal device and methods for producing same. The rim designs of the present invention improve, among other characteristics of the rim, structural durability, manufacturability, ease of insertion, comfort in use, and ease of removal of intravaginal devices. These designs incorporate one or more recesses in the inner portion of a rim piece that provide an attachment site for a separate dome piece. Attachment within a recess shields the exposed outer edge of the dome material from contact with epithelial surfaces and improves comfort and safety. In certain embodiments of the invention, a thinned inner portion of the rim serves as a handle that can be easily grasped by a finger to remove the device from the vagina. These devices are useful in providing a protective cervical barrier for contraception and disease prevention, to deliver beneficial agents, and as a means to collect and remove substances from the vagina. | 0 |
BACKGROUND INFORMATION
[0001] 1. Field of the Invention
[0002] The invention relates to the field of locks with keys. More particularly, the invention relates to a method of coding a key and a female lock part.
[0003] 2. Discussion of the Prior Art
[0004] In a key transfer system, the lock stamp or female lock part is built into the lock of the key transfer system and is therefore an integral component of the system, whereby a key is needed to open the lock and thereby the female lock part. The individual locks are provided with a unique coding between the female lock part and the key, so that it is only possible to operate the lock with a key having the matching code. Normally, the key meshes into the female lock part of the lock and thus creates a form-fitting unit. The female lock part itself works, for example, together with a blocking arrangement of the tumbler, or via an integrated square edge or something similar, for example, with an electrical switch.
[0005] An example of the prior art is shown in FIG. 1 . The coding comprises a combination of pins and boreholes. The key has a number of boreholes in a given arrangement, and the lock stamp is provided with an identical number of pins in the same arrangement as that of the key, which, when the codes match, can mesh into the boreholes of the key. The key can then be inserted far enough into the lock to operate the lock. It is not possible to operate the lock, if the hole and pin patterns do not match.
[0006] The prior art also teaches that, instead of pins and boreholes, milled letters or combinations of letters can be provided as key coding. Milled or cast contours are also used.
[0007] Characteristic for the prior art and the conventional codings is that the codings must be manufactured separately for the keys and the lock stamps. This means that the key is coded, for example, by machining the bores, and that the female lock part is made to match the key, by machining the bores and pressing in the pins.
[0008] It is obvious that the manufacturing these known codings is costly and that the number of codings is limited.
BRIEF SUMMARY OF THE INVENTION
[0009] It is an object of the invention to propose a method for manufacturing the coding in one production step and in both components at the same time, namely, in the key and in the lock stamp or female lock part or in each of two coding disks that are then affixed as coding faces to the key or the female lock part.
[0010] To achieve this object, it is recommended that a bolt-like blank, for example, be separated into two parts by a separating cut that is guided perpendicular and also parallel to the longitudinal axis of the blank, wherein the two parts are then post-processed to create the key and the female lock part, or are affixed as coding disks to a key and an female lock part. The separation plane between the two parts of the blank, which is created by the separating cut or the separating method, automatically forms the coding. The separation cut may be guided in such a way that that an angular or a wavy separation plane is created. In like manner, it is possible to provide a parallel or radial separating cut. Variations in the detail, the contour, the alignment of the contour, and the radial alignment of the contour to the longitudinal axis of the blank allow the maximum possible number of codings.
[0011] The coding disks thus created are connected to the actual key and the lock stamp, and the thus created and coded female lock part is built into the lock.
[0012] Instead of providing the coding directly on the components that are the key and the female lock part, it is also possible to separate a component into two parts, using the separation cut according to the invention that creates the matching coding on both parts, and then using the two parts as coding disks, one disk of which is then affixed to the key part, and the other to the female lock part.
[0013] If the coding is provided on the key and the female lock part, the coding of must be accomplished before the lock device is assembled. Because the coding has to be unique, this means that the coding can only be done per order. This makes the production of the lock very time-consuming.
[0014] It is possible, however, using the method according to the invention, to provide two coding disks that are then connected or affixed to the key and the female lock part. This makes it possible to provide the coding disks as the last step in the lock production process. It is now possible to manufacture and prefabricate the components of the lock, i.e., the key, the locking mechanism, the tumbler, the lock, and the like, and, separately, to manufacture coding disks. When an order is placed, the coding disk are then affixed to the key and the female lock part.
[0015] There are many suitable ways of connecting or affixing the coding disks to the key and to the female lock part, such as, for example, a positive form fit, material-joined, and interference fit. A crimp connection, a rivet connection, a screw connection, or a method using clips may be used. Means, such as safety latches or the like may also be used.
[0016] According to the invention, a key bolt with a key bit that extends through the female lock part may be inserted in the key, so that, in its operating state, e.g., when it is turned in the female lock part or in the lock, the key is prevented from being removed axially.
[0017] The blank may be made of metal or plastic and, for example, may be a precision-cast component or made of cylindrical or polygonal bar stock.
[0018] A laser separating method or a water-jet separating method are options for the separating method, although the invention is in no way limited in this regard.
[0019] In summary, the method according to the invention allows the key and female lock part, or a blank that is inserted between the key and the female lock part, to be coded in one production step on one initial component. Tolerances no longer have to be considered because the two coded parts always match, because they have been produced by the same separation cut.
[0020] The method according to the invention makes a very high number of codings possible, and the codings form parts that are created of a single material. This largely eliminates corrosion problems between the parts.
[0021] It is possible to create the lock codings, even with materials that are mechanically difficult to machine, and based on the selected separation method, to significantly reduce manufacturing costs.
[0022] Finally, it should be mentioned that, with the method according to the invention, neither scraps nor waste accrue.
BRIEF DESCRIPTION OF THE DRAWINGS
[0023] An embodiment of the invention is described below using the drawings.
[0024] FIG. 1 illustrates the prior art, a blank.
[0025] FIG. 2 illustrates the two individual parts manufactured from the blank by means of a separating method.
[0026] FIG. 3A illustrates a key with one type of coding.
[0027] FIG. 3B illustrates a female lock part with mating coding for key in FIG. 3A .
[0028] FIG. 4A illustrates a key with a pie-shaped coding.
[0029] FIG. 4B illustrates a female lock part with pie-shaped coding.
[0030] FIG. 4C illustrates a key with a continuously curved coding.
[0031] FIG. 4D illustrates a female lock part with continuously curved coding.
[0032] FIG. 5 illustrates a key and a female lock part manufactured according to the invention.
[0033] FIG. 6 is a plan view of the arrangement according to FIG. 5 (in the direction of arrow A).
[0034] FIG. 7 illustrates the use of coding disks.
DETAILED DESCRIPTION OF THE INVENTION
[0035] The present invention will now be described more fully in detail with reference to the accompanying drawings, in which the preferred embodiments of the invention are shown. This invention should not, however, be construed as limited to the embodiments set forth herein; rather, they are provided so that this disclosure will be complete and will fully convey the scope of the invention to those skilled in the art.
[0036] FIG. 1 illustrates the prior art, a key A and a lock stamp B, whereby the key A is provided with boreholes into which the pins that are arranged on the top of the lock stamp or key plug B can mesh. The coding is created the specific arrangement of the pins and the boreholes. It is obvious that both parts require a significant amount of machining for this type of coding: bores have to be machined in the key and the pins that fit into the bores have to be machined on the plug. The disadvantages of machining are known. For example, tolerances have to be maintained and that may be complicated by the fact that various materials may possibly be used, particularly for the pins that are provided in key plug B. Furthermore, machining is costly.
[0037] FIG. 2 shows a blank 1 that is a cylindrical bolt and that serves as the basis for the manufacturing of a lock stamp or female lock part 3 and a key 2 . FIGS. 3A and 3B show the blank 1 divided into two parts 1 A and 1 B, the two parts having a separation boundary T-T that forms the key 2 and the lock stamp 3 , respectively, on the two parts. The separation boundary T itself constitutes the coding and there are multiple ways of creating the coding. For example, as shown in FIGS. 3B and 4B , the separation process is carried out such that the separation boundary T-T is angular with planes that extend in directions both transverse and parallel to a longitudinal axis L-L of the blank 1 , so as to form a straight-edged and flat-planed array of coding elements. FIG. 3B illustrates such a separation. FIGS. 4A and 4B illustrate a separation boundary that creates coding elements that are variously raised segments, similar in shape to slices of a pie. FIGS. 4C and 4D illustrate coding elements that have a rounded or undulating contour. The center axis of the workpiece for creating all of these separation boundaries T-T must be focused, i.e., clearly defined, and the lock stamp 3 provided with a central borehole 7 as a runout.
[0038] As shown, the separation boundary T-T may have angular or rounded contours, whereby the angular contours are very well suited not only for providing the coding, but also for transmitting the torque between the key and the female lock part. The rounded contours are advantageous in that they are less prone to becoming dirty and pose a lower risk of injury, have, however, the disadvantage that they require an additional functional element for transmitting torque from the key 2 to the lock stamp 3 . FIG. 5 illustrates a key bolt 4 with a key bit 5 that is suitable for transmitting torque.
[0039] FIGS. 5 and 6 illustrate a ready-to-use component that comprises a key bow or grip 6 that is made of the same material as the key 2 or is firmly affixed to the key 2 . The separation boundary T-T between the key 2 and the female lock part 3 is constructed according to one of the previously described methods with the coding. The key bolt 4 with key bit 5 is inserted into the key 2 , into a borehole 10 that opens at a lower end of the female lock part 3 . The key bit 5 engages in a corresponding key slot 8 of the lock stamp 3 , thereby creating a highly rotationally rigid connector for transmitting torque between the key 2 and the female lock part 3 . Turning the bit 5 also locks it into a key recess 9 , so that the key bolt 4 is secured in place.
[0040] FIG. 7 illustrates one possible embodiment with coding disks 11 and 12 , which are affixed to the key 2 and the female lock part 3 , respectively, by conventional means, for example, by means of clips, a crimp connection, a rivet connection, a threaded connection, or locking rings, etc. FIG. 7 shows the actual key, designated with number 6 a, the coding disk 11 assigned to this key 6 a, and the female lock part 3 a with its associated coding disk 12 . The female lock part 3 a, the coding disks 11 and 12 , and the actual key 6 a have a through borehole 10 a into which, as previously described, a key bolt 4 a is insertable.
[0041] This embodiment with coding disks 11 and 12 has the advantage of making it now possible to pre-fabricate the components that form the locking mechanism, namely, the key 2 , the lock device, the tumbler, the lock elements, or the switch device, and then to fabricate the coding disks 11 and 12 , which then must be connected to the other components, only when an order is placed. Thus, upon receiving an order for a lock, only the coding has to be created, whereas the other components are prefabricated.
[0042] It is understood that the embodiments described herein are merely illustrative of the present invention. Variations in the method of coding the lock may be contemplated by one skilled in the art without limiting the intended scope of the invention herein disclosed. | A method for coding a key and a female lock part for a lock in a lock system, whereby a blank is separated into two parts by a separating cut that is guided perpendicular to the longitudinal axis and in the direction of the longitudinal axis of the blank. The cut forms a coding contour. The two parts are then post-processed to form the key and the female lock part or serve as coding disks that are affixed to a key and a female lock part. | 1 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a device for reducing or preventing snoring and, in particular, to an anti-snoring device which can be easily fit to patients having either a wide or a narrow dental arch.
2. Description of the Related Art
Snoring is normally the result of vibration of the uvula, soft palate, and adjacent structures during sleep and signals partial obstruction due to the narrowing of the upper airway at that site. In most cases, breathing is normal or only minimally impaired, and symptoms primarily concern sleep disturbance and the social consequences of snoring. In other cases, snoring is associated with the obstructive sleep apnea syndrome, a serious condition characterized by intermittent upper airway obstructions that require arousal for relief.
Various devices are known in the art for placement in the oral cavity and intended for to reduce snoring. Some investigators have provided devices which are arranged to seal the lips of the wearer, one to another, thus blocking air passage through the mouth. Others have recognized that portions of the uvula, soft palate, and adjacent structures vibrate during sleep, in response to the passage of air past these tissues, and attempt to minimize such vibrations by providing devices which sharply reduce the volume of air passing through the mouth, without necessarily completely blocking the mouth. However, if the nose is blocked, or partially blocked, this reduction of the airway increases the velocity of the air passing those tissues and snoring can actually increase.
Yet another type of prior art device is exemplified by the device of U.S. Pat. No. 1,674,336 to King. King intends that his device will maintain a plentiful supply of oxygen to the blood of a user during sleep, and even reduce snoring. His structure comprises an upper channel and a lower channel to receive the upper and lower teeth, respectively. The two channels are spaced apart vertically to prop the upper and lower front teeth apart and to define an air passage therebetween. Thus, in use, the device props the teeth of a user apart in a fixed position, which King claims opens the posterior airway to facilitate the passage of air to and from the throat and lungs. As the device receives the top and bottom teeth and fixes their relative position, natural mouth motions, including motion of the lower jaw, are prevented.
A device which effectively alleviates or prevents snoring is disclosed in my earlier U.S. Pat. No. 5,092,346 for a Dental Orthosis for Alleviation of Snoring, marketed under the name Snore Guard®, the disclosures of which is incorporated herein by this reference. That structure includes an upper portion in the form of pair of parallel and substantially coextensive walls defining a trough corresponding in shape to the curvature of the patient's upper dental arch, for receiving the upper teeth of the patient. Once properly fitted, the device will snugly receive the front teeth and the premolars and remain positioned independent of natural motions of the lower jaw.
The lower portion of the '346 patent device is formed into a ramp structure whereby natural jaw motions result in the engagement of the lower teeth against the ramp, which will cam the lower jaw into a more forward position. An aperture in the device between the upper and lower portions facilitates the passage of air for mouth breathing and attracts the tongue forward. By inducing the lower jaw and tongue to a more forward position, the device induces a more open posterior airway in the patient, resulting in a significant reduction in snoring.
In contradistinction to the teachings of King, the structure of the '346 patent device does not fix the position of the upper and lower jaw and tongue. Instead, by an adroit arrangement of the structure, the device snugly attaches to the upper teeth and jaw, while allowing natural mouth movements including motions of the lower jaw and teeth, and tongue. That device is further distinguished in providing the ramp to engage the lower anterior teeth and induce forward movement of the lower jaw, resulting in the opening of the posterior airway.
SUMMARY OF THE INVENTION
Thus, the '346 patent device was a significant improvement in the art over devices of the type disclosed in King. That is not to say, however, that improvements in the '346 patent device are not possible, and, in fact, the present invention constitutes an improvement in that device.
More particularly, I discovered that, because the '346 patent device provided substantially co-extensive upper trough defining walls which were curved to accommodate the patient's dental arch, a particular configuration of the device may only be fit to a certain range of dental arch sizes and shapes. Thus, custom molding of the device and/or maintenance of a relatively large inventory of the '346 device may be required to accommodate a variety of patients.
Thus, it was an object of the invention to provide an anti-snoring device generally of the type disclosed in the '346 patent, but which could accommodate a variety of dental arch sizes and shapes so that a single size or a few sizes can accommodate all users, thereby eliminating the need for a large inventory and the time and cost of custom fitting.
The foregoing object is achieved in accordance with the invention by providing a device having an upper portion which is defined by an arching front wall and a truncated rear wall which is substantially parallel to the front wall but which extends through an arch substantially smaller than that of the front wall. I found that a reduction in the rear wall of the upper trough allowed a device of a given size to be fit to patients having a variety of dental arch sizes and shapes. Further, I found that, surprisingly, despite the significant reduction in the arch length of the rear wall of the upper trough, a snug fit, irrespective of the dental arch, was possible and the device could still remain positioned independent of natural motions of the lower jaw. Thus, like the '346 device, the ramp structure of the lower portion of the device allows natural jaw motions, including the bite reflex and, upon engagement of the user's lower teeth against the ramp, will cam the lower jaw into a more forward position, thereby achieving the advantages of that structure. However, because the device disclosed hereinafter does not require custom fitting to the upper portion to the patient's dental arch, the device can accommodate the physiology of a variety of patients.
Other objects, features, and characteristics of the present invention as well as the methods of operation and functions of the related elements of structure, and the combination of parts and economies of manufacture, will become more apparent upon consideration of the following description and the appended claims with reference to the accompanying drawings, all of which form a part of this specification, wherein like reference numerals designate corresponding parts in the various figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view from the rear of a dental orthosis provided in accordance with the invention with the resin material omitted from the tooth receiving trench, for clarity;
FIG. 2 is a side elevation of the device of FIG. 1 with the resin material omitted from the tooth receiving trench, for clarity;
FIG. 3 is a perspective view from the forward side of the device of FIG. 1 with the resin material omitted from the tooth receiving trench, for clarity;
FIG. 4A is a cross-section side view of the device of FIG. 1;
FIG. 4B is a view similar to FIG. 5A, showing an impression made by a patient's teeth once the device has been fitted to that patient.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
As illustrated in FIGS. 1-5, the dental orthosis 10 for reducing snoring in accordance with the present invention comprises a structure shaped to generally conform to the upper dental arch of a user and extending at least between the pre-molar teeth on each side of the wearer's mouth.
The main body 12 of the device may be formed from a single piece of methylmethacrylate, which is a plastic material used for dentures. If formed of methylmethacrylate, the device must then be cured to prevent absorption of mouth fluids, or cleaning fluids, and to present a smooth non-irritating surface to the soft tissues of the mouth.
However, the main body 12 of the device is most preferably composed of a resilient semi-rigid polycarbonate resin thermoplastic having good physical characteristics and having a specific gravity of about 1.20, a tensile strength (yield) of about 9000 and a softening temperature of about 310 degrees F. An example such resin is sold by the General Electric Company under the Registered Trademark LEXAN. The material provides a framework for the device, and it is preferably used in conjunction with an additional resin material as further discussed below.
In the preferred embodiment, a substantial advantage to the user is offered when another resin layer 14, 16 is bonded to the polycarbonate resin thermoplastic device described above, such layer 14, 16 preferably composed of an ethylene-vinyl acetate copolymer resin having a softening and molding temperature of between about 125 and 175 degrees F and most preferably about 150 degrees F. An example of such resin is sold by Du Pont Company under the Registered Trademark ELVAX.
As will later be more fully explained, the preferred embodiment is self fitting, for both narrow and wide arches, so that one size of the device will accommodate all or substantially all users. This saves time and money as no custom molding and fitting is required, thereby eliminating the need for a variety of molds and the services of a dental laboratory in fitting the device to a particular patient.
Considering now FIGS. 1 and 2, the dental orthosis 10 comprises a semicircular structure, more specifically an arch, having an outer or forward wall 18 corresponding generally to the curvature of an upper dental arch, and a truncated rearward wall 20, which define therebetween a teeth receiving trench 32. In the illustrated embodiment, truncated rearward wall 20 has an upper edge of about 15 mm in arch length and a lower edge portion adjacent the base of the trough of about 25 mm in arch length. The rearward side edges are inclined downwardly from the upper edge to the lower edge portion at an angle of 45 to 60 degrees to intersect with ends 22.
A ramp structure 24 extends laterally between the lower extremities of wall 12. The ramp structure includes a ramp element 26 defined as a portion of the main body 12 which extends rearwardly at an angle of about 60°.
An aperture 28 extends through the device as detailed below. The bottom 30 of the trench 32 is substantially horizontal when the device 10 is in use.
More particularly, in order to form a more generous air passage 28 a pair of stanchions 34 join the ramp element 26 to the upper portion of the main body. The ramp element 26 may be configured as deemed necessary or desirable for ease of application and durability of the acetate copolymer resin layer 14. In the alternative, the ramp element 26 has uniform upper and lower surfaces. An aperture, or a series of apertures may be provided to facilitate the application of the resin layer 14 to increase its durability on the structure.
The resin layer previously described is shown by reference to FIGS. 4A and 4B, which is a cross section of the device of FIGS. 1-4. A layer of acetate copolymer resin 16 is shown applied to the teeth receiving trench 32 and to the ramp element 26. FIG. 4B is the same cross-sectional view as found in FIG. 4A. The only difference is that FIG. 4B shows a tooth impression 36 in the acetate copolymer resin layer resulting from the fitting of the device to the patient.
The lower anterior teeth of the user engage the device only at a ramp surface of ramp structure 24 whereby natural lower jaw and teeth motions are preserved. Thus, the lower anterior teeth naturally engage the ramp structure 24 and are induced by natural jaw movements to advance along the ramp structure 24 moving the lower jaw into a more forward position.
When the device is formed from the polycarbonate resin-thermoplastic having the layer of acetate copolymer resin bonded thereto at the teeth-engaging surfaces, namely the trench which receives the upper teeth and the ramp which receives the lower teeth, then individual fitting of the device to the user is greatly simplified, as is user comfort. The acetate copolymer resin layer 16 is about 3 to 4 millimeters in thickness in the trench 32 and a coating 14 of approximately 2 to 3 millimeters thick is applied to the ramp element 26. The acetate copolymer resin has a substantially lower softening and molding temperature than that of the polycarbonate resin-thermoplastic forming the main body of the device and thus individual fitting to the user's mouth is simplified. An immersion of the device in a hot fluid, preferably water, prior to the fitting serves to soften the acetate copolymer resin layer whereby it accepts the users distinctive tooth configuration during the fitting process. Upon cooling to ambient temperature, the acetate copolymer resin retains the user's tooth configuration, for ease of repeat placement by the user. Excess resin can be cut from the device to make the device more comfortable to use. Additional minor adjustment may be advisable to increase comfort for the user or to modify the alignment of the device. If extensive dental work is later performed or if mechanical damage occurs, a new fitting may be necessary for mechanical comfort and ease of use.
It is also important to note that relatively minor forward movement of the jaw, in the range of 2 to 6 mm, serves to reduce the incidence of snoring. As is the case with any orthosis, further adjustment of the device to the user may be desirable from time to time.
Considering again the Figures the dental orthosis comprises a semicircular structure, more specifically an arch, comprising a front wall 18 and a truncated rear wall 20. The front and rear walls are essentially parallel. In order to accommodate users having a variety of dental arch shapes and widths, rear wall 20 has an arch length substantially less than that of wall 18. As is apparent from the foregoing and as can be seen from FIG. 1, in particular, to achieve the objects of the invention, the angle transcribed by the rear wall is substantially less than the angle transcribed by the front wall. Thus, the rear wall lies behind the front teeth and the front teeth are snugly received between the front and rear walls, preferably in the relatively soft filler material 16, as described above. The rear wall terminates laterally, rearwardly in edges which slope downwardly at an angle of about 45 to 60 degrees to intersect ends 22, as noted above. The device can thus be fit to a patient substantially irrespective of the disposition and arch of the patient's upper teeth rearwardly of the front teeth and, substantially irrespective of the curvature of the user' s dental arch, the device will be snugly retained in proper position in the mouth.
In accordance with the invention, then, with only a single or relatively few sizes in inventory, the device can be fitted to the patient by a dentist in a matter of minutes. With proper instructions and safeguards, the device could also be self-fitted by the patient.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. | A dental orthosis is provided for use in the treatment of snoring. The upper portion of the device defines a trough for receiving some of the upper teeth of the patient. The rear wall of the trough is truncated so that the device can accommodate both narrow and wide dental arches so that one size of the device can accommodate substantially all users. Once inserted into the mouth the device snugly engages the upper teeth, particularly the front teeth, and remains positioned independent of natural motions of the lower jaw. The lower portion of the device is formed into a ramp structure whereby natural jaw motions result in the engagement of the lower teeth with the ramp, which will cam the lower jaw into a more forward position. | 8 |
BACKGROUND OF THE INVENTION
In the circular stack sheet feeding device according to West German Pat. No. 2,521,849, the areas of the support which determine the position of the sheet stack define a single plane. As long as the sheet stack has its full thickness or height, it is thereby assured that the uppermost sheet of the stack will lie in the plane defined by the two rollers and thereby be reliably taken hold of by the individualization means because accordingly the support only contacts the imbricated end of the stack. Toward the end of the stack, however, the thickness decreases. Because in the sheet feeding device according to the cited patent, the support for the end with the decreasing stack thickness is automatically pivoted into a position assuming a corresponding lower inclination, the sheet stack comes into contact with the support-also in the area of its underside following the imbricated end - which results in a bend being formed across the upperside of the stack. This bend results in the respective top sheet no longer lying in the plane defined by the rollers. This result can lead to malfunctions at the stack end in the sheet feeding device, manufactured according to the cited patent, in the removal of the uppermost sheet by the individualization means.
SUMMARY OF THE INVENTION
The primary purpose of the present invention is to improve a circular stack sheet feeding device with the view in mind that the sheet of a stack end can also be freely taken hold of by the individualization means. This object is obtained, according to this invention, because the support is divided into two sections which are pivotable relative to each other about a fold axis which lies across the direction of transport of the conveyor belt guided thereover. These two sections are capable of being set in pivotable positions and the angle defined thereby is 180° or an upwardly open obtuse angle.
The division of the support into two such sections and the pivotability of these sections relative to each other enables the support to form not only the primarily even surface for the sheet stack necessary for normal stack thicknesses, but also an angled support surface in the area of the folding axis. With this type of support surface, as the thickness of the stack decreases toward the end of the stack, the forming of a bend or kink in the upper side of the stack is avoided because the support assures that the bend in the underside of the stack is at the transition to the imbricated end. The kink is formed automatically when the stack thickness is kept full in the area of the folding axis by the bend in its support surface. This result is achieved because one section holds the imbricated section and the other section holds the non-imbricated underside of the stack in the correct angular positions to each other. Accordingly, the respective top sheet of the end of the stack is forced to lie in the same plane as the respective top sheet of the sheet stack at full thickness.
In many cases it will be sufficient to arrange the folding axis beneath the individualization means, which may take the form of a suction wheel. If it must be taken into consideration that the transition point of the nonimbricated underside of the sheet stack to the imbricated end can clearly deviate from the position lying beneath the individualization means, then the folding axis would have to be provided with means to allow shifting in a horizontal direction across its longitudinal dimension. This shifting could be carried out, for example, by a telescopically extending embodiment of the two sections.
The adjustment of the sections of the support, which sections are pivotable relative to each other, is possible in various ways while the stack thickness is reduced at the end of the stack. One effective manner is to provide a motor drive for the adjustment device in order to be able to automatically perform the adjustment without interrupting operations. For example, one can arrange a pivot drive for the one section at the other section. Such a drive could connect the two sections in a pivotable manner with selectable pivotable positions with the aid of articulated fittings. One can also, however, connect the section of the support farthest removed from the reversing drum with the other section in a freely pivotable manner by means of the folding axis, said support being supported in the area of its free end. In this case, the folding axis can be associated with a height adjusting mechanism, whereby the angle which the two sections together define can be changed by a height adjustment of the folding axis. Thus, the end of the support facing the reversing drum is pushed upward, for example, with the aid of springs. One can also form the folding axis as the pivot axis of the support and provide it with a pivot mechanism with a drive in place of one or more springs. However, in this type of embodiment, it is advantageous to make a height adjustment of the folding axis to varying stack thicknesses.
Because the position of the uppermost sheet changes as the thickness of the stack decreases, in a preferred embodiment, a sensor is arranged above the removal platform. This sensor is capable of detecting a deviation of the top sheet from the correct level. The monitoring thus need not be performed by an operator. Preferably, this sensor is formed as a control switch with a feeler which controls the adjusting mechanism or mechanisms. The support can then be automatically brought from the fully extended position into the location and angular position corresponding to the decreased stack thickness.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention is described below in greater detail with the aid of exemplary embodiments illustrated in the drawings. Shown in schematic and partial view are the following:
FIG. 1 is a side view of a first exemplary embodiment in a position of the support with a normal stack thickness;
FIG. 2 is a side view of the exemplary embodiment according to FIG. 1 in a position of the support fully extended with a decreased stack thickness;
FIG. 3 is a side view of the first exemplary embodiment in a position of the two sections of the support defining an obtuse angle for an increased stack thickness;
FIG. 4 is a side view of a second exemplary embodiment in a position of the two sections of the support defining an obtuse angle; and
FIG. 5 is a side view of a third exemplary embodiment in a position of the two sections of the support defining an obtuse angle.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A circular stack sheet feeding device, with the aid of which sheets can be individually led to a processing machine, particularly a folding machine, has a machine frame 1 which supports a loading platform 2 arranged above the machine frame 1. The free end of the loading platform 2 is located near a first diverting roller 3 and the opposite end is located near a second diverting roller 4. A rigid support plate 5 is attached to the diverting roller 4. The plate 5 ends below a reversing drum 6 rotatably mounted in the machine frame 1. On the opposite end of the plate 5, the second diverting roller 4 has an axis lying across the direction of delivery, which axis is pivotably mounted. In the exemplary embodiment, this pivot axis coincides with the axis of rotation of the diverting roller 4. Near to the end of the support plate 5, lying beneath the reversing drum 6, at least one biased pressure spring 22 engages on the underside thereof and is connected on the other end to the machine frame 1. The force of this pressure spring 22 is adjusted in such a manner that the support plate 5 remains in contact with a plurality of conveyor belts 7 which run for a distance spaced from each other over the first diverting roller 3, the loading platform 2, the second diverting roller 4 and the support plate 5, and then around the reversing drum 6 up to a third diverting roller 8 which is arranged at a distance above said reversing drum 6, form where the conveyor belts 7 return to the first diverting roller 3 by means of further diverting rollers (unnumbered), of which one acts as a tension roller and at least one other acts as a drive roller.
At a distance above the support plate 5 at a height which is adapted to the height of the transport path to the subsequent processing machine, a removal platform 11 is arranged, the free end of which is formed by a diverting roller 12 that lies above the edge zone of the loading platform 2 adjacent the second diverting roller 4. A plurality of adjacent conveyor belts 13 which are arranged at a distance spaced from each other are guided over the diverting roller 12 and run from the diverting roller 12 over a spring loaded tension roller 14 to the reversing drum 6. The conveyor belts 13 wrap partially around the reversing drum 6 and then run back to the diverting roller 12. These conveyor belts 13 form the contact surface for the removal platform 11. In addition, the removal platform 11 has two rollers 15 and 16 which are arranged in a displaced manner in the longitudinal direction of the conveyor belts 13. The axes of these two rollers 15 and 16 lie parallel to the axes of the diverting roller 12 and the reversing drum 6. The upper side of the roller 15 which lies close to the diverting roller 12, and the underside of the roller 16, which is arranged close to the reversing drum 6, lie in the plane in which the respective front sheet of the imbricated sheet stack transported from the loading platform 2 to the removal platform 11 by the conveyor belts 7 and 13 as well as by the reversing drum 6, is intended to lie. In the exemplary embodiment, as is common, this plane is a horizontal one.
The two rollers 15 and 16 are not only rotatable, but are also shiftable in a lateral direction relative to their longitudinal axis in the plane defined by them for the top sheet. In the exemplary embodiment, said shifting is necessarily in the same degree and in opposite directions. This is achieved by an adjusting transmission which is not shown.
At least in the region between the rollers 15 and 16, the end of the stack is supported by a support 23, embodied as a support plate, which forms a contact surface for all conveyor belts 13. The support 23 is divided transversally relative to the direction of movement of the conveyor belts 13 into two sections 23' and 23". These two sections 23' and 23" are pivotably connected with each other at a separation line by a folding axis 30 which lies across the direction of movement of the conveyor belts 13. The folding axis 30 is rotatably mounted in the section 23' in the exemplary embodiment and is rigidly connected with the other section 23" by mounting elements 31. See FIG. 3. The one laterally extending end of the folding axis 30 is coupled with a self-locking miter transmission gear 32, which is capable of being selectively driven in one or the other direction by an electric motor 34 through a drive shaft 33. A rotation of the folding axis 30 results in a change of the angle, which the two sections 23' and 23" define between themselves.
As shown in FIG. 1, the end of the section 23" of the support 23 adjacent the roller 15 is pivotably mounted about an axis lying across the direction of movement of the conveyor belts 13. Thus in this exemplary embodiment, the support 23 is pivotably mounted about the axis of the roller 15. In addition, draw springs 28 engage the sides of the support 23. The other ends of the springs 28 are connected to the axis of the second roller 16. The force of the draw springs 28 is selected in such a manner that the section 23" adjusts to an angle which results in the top sheet assuming a horizontal position in the plane determined by the rollers 15 and 16. Slightly horizontal plane is an individualization means in the form of a suction wheel 19 which takes hold of the top sheet and removes it across the direction of movement of the conveyor belts 13.
In this exemplary embodiment, the folding axis 30 lies beneath the suction wheel 19. It can, however, be brought into a position laterally displaced from this position if the shape of the sheet stack requires it, because both the section 23' and the section 23" are formed so as to be telescopically extensible.
FIG. 1 shows the position of the support 23 with a full thickness or height of the sheet stack. Toward the end of the stack, however, the stack thickness decreases, as shown in FIG. 2. If one were to maintain an angle of 180° between the two sections 23' and 23", as the stack thickness decreases, as shown in FIG. 2, this arrangement would result in a bend at the transition to the imbricated end of the cable on the underside thereof, which bend would increasingly disappear and, instead of a bend on the underside, a bend on the upperside of the stack would result. The top sheet would then no longer be found in the horizontal position which is necessary for a reliable removal by means of the suction wheel 19.
In order to prevent the upperside of the stack from being deformed in the above-described manner as a result of the decreasing stack thickness, the angle between the two sections 23' and 23" is decreased to the necessary degree. The angle to be established is determined by the angle described by the imbricated end of the stack with the adjacent, non-imbricated underside of the stack. With the corresponding adjustment of the angle between the two sections 23' and 23", as well as with the corresponding positioning of the bend of the support 23 of the transition at the non-imbricated underside of the stack to the imbricated end as the stack thickness decreases, the section of the stack adjacent the imbricated end is supported by the section 23' of the support 23 in the angular position which is correct with regard to the imbricated end, whereby the position of the top sheet of the stack remains unchanged with regard to the suction wheel 19, despite the decreased stack thickness.
In order to be able to automatically undertake the change of the angular position of the two sections 23' and 23" relative to each other, a vertically shiftable feeling rod 35 is arranged adjacent the suction wheel 19, in such a manner as to cooperate with and activate a control switch 36 when the top sheet of the stack assumes a position which deviates upward from the predetermined horizontal poistion. The control switch 36 is thus only turned on when the bend shown in FIG. 2 begins to form on the top side of the stack. The control switch 36 then turns on the electric motor 34 which rotates in a direction which results in an upwardly open obtuse angle being formed between the sections 23' and 23" of the support 23. As soon as the top sheet has again reached its correct horizontal position because of the forming of the bend in the support 23, the control switch 36 turns the electric motor 34 off. As shown in FIG. 3, the self-locking miter transmission gear 32 maintains the two sections 23' and 23" in the achieved angular positon. The remaining sheets of the stack can then be removed by means of the suction wheel 19 without difficulty. Should a correction of the angle between the two sections 23' and 23" be necessary again because of further decreasing stack thickness, this will also take place automatically with the aid of the feeling rod 35 and the control switch 36 as well as with the aid of the electric motor 34. The change of the angular position between the two sections 23' and 23" has no influence on the function of the draw springs 28.
The second exemplary embodiment illustrated in FIG. 4 is distinguished from that according to FIGS. 1-3 only by a different embodiment of the support 123 which corresponds to the support 23 of the first exemplary embodiment. The remaining portions of the circular stack sheet feeding device are therefore not explained in detail. To that extent, the reader should refer to the statements regarding the first exemplary embodiment according to FIGS. 1-3.
The support 123 is divided, across the direction of movement of the conveyor belts 113 which are guided thereover, into two sections 123' and 123", which sections are pivotably connected with each other at the line of separation by a folding axis 130. At both sides of the support 123, namely in this exemplary embodiment, at the ends of the folding axis 130, there is attached the upper end of a stroke device 137, whose other end is connected to the machine frame 101. These two identical stroke devices 137 are, in this exemplary embodiment, hydraulic cylinders. But other means, such as hoisting spindles driven by means of an electric motor, could also be used.
As in the first exemplary embodiment, draw springs 128 engage at the section 123 at the free end thereof near the reversing drum 106. In addition, the section 123" is pivotably mounted on the axis of the roller 115 at its free end, in a manner similar to that of the section 23". The axis of the roller 115 is adjustable in the horizontal direction by means of an adjusting drive (not shown) to the same degree as the roller 116, but in the opposite direction. This adjustment is possible as a result of the telescopically extensible embodiment of the two sections 123' and 123" without a shifting of the folding axis 130. The telescopically extensible embodiment of the two sections of the support 123 also makes possible a shifting of the folding axis 130 in the horizontal direction. In case this type of shifting is necessary to adapt the support 123 to the bend in the underside of the stack at the transition to the imbricated end, it is practical to hinge the lower end of the hoisting devices 137 to a horizontally adjustable sled (unnumbered) or the like.
The hoisting devices 137 are controlled by a control switch 136, which is arranged at a distance above the top sheet that is to be taken hold of by the individualization means 119. The control switch 136 is activated by means of a feeler rod 135, which detects the position of the top sheet of the stack. The control switch 136 causes a lowering of the folding axis 130, when the top sheet lies above the horizontal plane in which it must be located for a smooth removal by the individualization means 119. Thus, it is assured that the two sections 123' and 123" are brought into a position in which they define an upwardly open obtuse angle when the stack thickness decreases at the end of the stack. The control switch 136, however, causes a lifting of the folding axis 130 if the top sheet lies too low below the horizontal plane in which the top sheet must be located for smooth removal. Thus, the angle of inclination of section 123" of the support 123 is automatically adapted with the aid of the control switch 136. The hoisting devices 137 are automatically adapted to the angle of inclination of the imbricated end of the stack with regard to the top side of the stack.
The third exemplary embodiment shown in FIG. 5 is also distinguished from the first exemplary embodiment according to FIGS. 1-3 only by a different embodiment of the support 123, so that with regard to the other characteristics of this circular stack sheet feeding device, the statements made with regard to the second exemplary embodiment according to FIG. 4 still hold.
The support 223 is divided into two sections 223' and 223" across the direction of movement of the conveyor belts 213 guided thereover. Both sections 223' and 223" are pivotably connected with each other by a folding axis 230. The folding axis 230 in this third exemplary embodiment also serves as a pivot axis for the section 223' and is therefore mounted in a stationary position in the machine frame. One can, however, arrange the position of the folding axis 230 in a height-adjustable manner in the machine frame and provide hoisting devices for this purpose as in the second exemplary embodiment according to FIG. 4. The effect achieved with a height adjustment of the folding axis 230 is the same as that in the second exemplary embodiment according to FIG. 4.
The section 223" is pivotably supported at one end on the folding axis 230 and is also pivotably supported in the area of its free end at the axis of the roller 215 which corresponds to the roller 15 of the first exemplary embodiment.
The section 223' has an extension passing beyond the folding axis 230, which lies below the section 223". This type of extension, not being an extension of the other section, could come into use also in the first exemplary embodiment according to FIGS. 1-3 if a differently embodied pivot mechanism were to be provided for the pivoting of the sections 23' and 23" of the support 23 relative to each other. A lever 238 is hinged to the extension of the section 223' with an axis parallel to the folding axis 230. This lever 238 is hinged on the other end to a horizontally shiftable sled 239. If the sled 239 is moved to the left as seen in FIG. 5, with the aid of a drive motor (not shown), then the section 223' of the support 223 is pivoted clockwise about the folding axis 230, without the section 223" changing its angle of inclination. The drive of the sled 239 is controlled by a control switch 236 and a feeler rod 235 associated therewith, which, like the control switch 136 and the feeler rod 135 next to the suction wheel 119, are arranged above the top sheet.
Initially, the section 223' is set at the same angle of inclination as the section 223", i.e., at the angle formed by the imbricated end of the stack. If the stack thickness begins to decrease, then as is shown in FIG. 2, a bend begins to form on the topside of the stack which results in a shifting of the top sheet upward toward the suction wheel 19. Control switch 236 reacts to this shifting and causes a movement of the sled 239 to the right as seen in FIG. 5. In this manner, the section 223" of the support 223 is pivoted counterclockwise, whereby the two sections 223' and 223" arrive at a position in which they define an upwardly open, obtuse angle. By means of this transition from the fully extended position into the position forming a bend, the bend in the upperside of the stack is eliminated. The top sheet can then continue to be drawn off without difficulty by the suction wheel 219 or by other individualization means. | The present invention relates to a circular stack sheet feeding device having a lower loading platform, which can be loaded with imbricated (arranged with regular overlapping edges) sheet stacks, having a transport and reversing mechanism, which transports the imbricated sheet stacks in a first transport direction to the underside of a reversing drum and with the aid of the reversing drum transports the sheets about the drum upwards in a second transport direction onto a removal platform, above which is guided an elastically yielding, taut conveyor belt which runs in the direction of delivery and runs between two rollers which are arranged on axes parallel to the reversing drum and are horizontally adjustable in the delivery direction of the delivery wheel. The underside of the roller lying closest to the reversing drum and the upper side of the other roller arranged in the area of the end of the removal platform opposite the diverting drum are adjusted to the same height. Individualization means remove the top sheet of the stack in a perpendicular direction from the transport direction of the conveyor belt. The conveyor belt is supported in the removal area between the two rollers by a rigid support divided into two sections which are pivotably mounted about an axis that lies in the axis of rotation of the second roller or is parallel thereto. At least one pivot mechanism engages and is capable of pivoting the rigid support about the first roller. | 1 |
This application is a national stage entry of PCT/US2011/020565 filed on Jan. 7, 2011 which claims benefit of U.S. provisional application 61/293,620 filed on Jan. 8, 2010. Both applications are incorporated by reference in their entirety.
TECHNICAL FIELD
The present invention is directed generally to antenna beam controlling systems and, more specifically, to antenna beam control elements, systems, architectures, and methods for radar and other applications, such as communication systems, etc.
BACKGROUND ART
Radio transmitter and receiver antennas are frequently installed at the side of towers, such as telecom and wind turbine towers, and other physical structures, as well as in the vicinity of other systems employing radio transmitters and receivers. Antennas with wide azimuth coverage or that may scan a wide azimuth range may get the physical structure inside its radiation area, where the structure may disturb the antenna function. In addition, antenna arrays often generate a desired main lobe, but also side and back lobes which may reduce the effective gain and directivity of the total array and produce undesired reflections, thereby diminishing the performance of the system.
While the physical structure itself will limit the useable azimuth angle for the antenna, even for azimuth angles outside the physically blocked sector, part of the antenna beam may illuminate the physical structure, reducing accuracy by undesired reflections via the structure, or the structure can produce secondary reflections even when it is not illuminated. Also, the antenna beam must not be pointed such that multipath interference via the structure may disturb the system function. For the antenna to operate at azimuth angles close to the structure, a high gain antenna is required. For an antenna with steered beam, scan angles close to the structure may not be useable. For low gain arrays, the useable scan angle becomes strongly limited due to the wide lobe and possible side lobes. Adding RF absorbing material at the physical structure will reduce the problem. However, as the tower structure may be very large compared to the antenna itself, adding absorber material to the structure itself may be expensive or impractical.
In addition, the proximity of other systems employing radio transmitters and receivers, such as radar and communications system, can limit the usable angle and/or bandwidth of a system. The neighboring radio based systems combined with physical structure interference can severely limit the operational range of antenna-based systems.
Prior art solutions to the problem of obstructions typically involve the use of directional antennas or absorbers. Directional antennas, such as horns, often provide for higher gain, but limit the coverage area of the antenna, thereby requiring more antennas to provide coverage and increasing the cost. The increased number of antennas may also make installation and operation of the antennas more difficult, if the antennas have to be aligned more precisely. The use of absorbers, such as those described in U.S. Pat. No. 5,337,066, reduces the gain of the antenna, which, in turn, typically reduces the coverage distance of the antenna.
Improved antenna solutions are required that overcome the various limitations associated with prior art solutions to enable systems with improved performance and applications.
SUMMARY OF INVENTION
The present invention provides, among other things, antenna beam control elements, systems, architectures, and methods for radar and other applications, such as communication, to improve transmit and receive performance of the devices and systems employing such antennas. A method of managing the impact of radiation reflected or emanating from nearby structures, radars, and networks, on low or high gain antennas has been found by providing one or more beam control elements that can be placed in the antenna near field to increase the antenna gain and enhance radiation emitted or received by the antenna at an angle less than a first angle relative to the antenna gain and radiation emitted or received by the antenna at an angle greater than a first angle. In various embodiments, the antenna gain and peak intensity at an angle less than the first angle can be increased and the antenna gain and peak intensity at an angle greater than the first angle can be decreased relative to antenna gain in the absence of the beam control element.
The present invention provides, among other things, antenna beam control elements, systems, architectures, and methods for radar and other applications, such as communication, to improve transmit and receive performance of the devices and systems employing such antennas. A method of managing the impact of radiation reflected or emanating from nearby structures, radars, and networks, on low or high gain antennas has been found by providing one or more beam control elements that can be placed in the antenna near field to increase the antenna gain and enhance radiation emitted or received by the antenna at angle less than a first angle relative to the antenna gain and radiation emitted or received by the antenna at angle greater than a first angle. In various embodiments, the antenna gain and peak intensity at an angle less than the first angle can be increased and the antenna gain and peak intensity at an angle greater than the first angle can be decreased relative to antenna gain in the absence of the beam control element.
Beam control elements can be deployed in combination with the antennas in various systems of the present invention such that the impact of reflected radiation from wind mill, communication, or other towers supporting the system or other nearby structures, as well as radiation from nearby wireless communication networks can be decreased to an acceptable level. The amount of reflected radiation from structures and radiation from nearby networks that is acceptable may depend upon the particular application in which the inventive system is deployed. For example, radar and voice and data mobile phone applications may have differing requirements for signal to noise ratio, as well as other signal characteristics.
The beam control elements can include absorbing and reflective material that are used in combination to improve the gain of the antenna, while reducing undesirable radiation from being transmitted and received by the antenna. The beam control elements can be positioned proximate to the antenna to be comparable in size with the antenna itself, which is beneficial from a cost and installation perspective. One of ordinary skill will appreciate that the impact of the beam control element on the signal/radiation pattern/antenna performance will be influenced by its location in the near field.
The applicable antenna may consist of one basic antenna element or 2 or more basic antenna elements in an array in horizontal (azimuth) and vertical (elevation) axes. The use of the present beam control element allows a wide antenna beam to be used, which is desirable for cost reasons, because the number of antenna elements can be reduced. The inventive wide area antenna with the beam control element with improved performance also provide additional margin in the installation and use of the antenna, because of increased coverage area and distance. In addition to fixed systems, the inventive beam control element is compatible with phase controlled antenna elements, which allows beam steering to be used, for example in electronically scanning radar applications, etc.
In this and other manners, the present invention addresses limitations of the prior art as will become further apparent from the specification and drawings.
BRIEF DESCRIPTION OF DRAWINGS
The accompanying drawings are included for the purpose of exemplary illustration of various aspects of the present invention, and not for purposes of limiting the invention, wherein:
FIG. 1 shows embodiments of an antenna system with at least one beam control element;
FIG. 2 shows embodiments of at least a portion of an antenna system with reference axis of radiation and beam control element;
FIG. 3 a & b show depictions of the selection of a first angle and placement of a beam control element relative to an antenna element, idealized main and side lobes, and a structure,
FIG. 4 shows 2×8 array embodiments from the back side with Z axis being the reference azimuth beam angle;
FIGS. 5-7 show various simulation and test results of antenna gain vs. azimuth angle with and without the beam control element of the present invention,
FIGS. 8 a & b show depictions of the placement of the antenna system in a wind mill application,
FIGS. 9 a & b show embodiments of the present invention used in communication and radar applications, and,
FIG. 10 shows alternative embodiments for deployment in various applications from a top view.
It will be appreciated that the implementations, features, etc. described with respect to embodiments in specific figures may be implemented with respect to other embodiments in other figures, unless expressly stated, or otherwise not possible.
DESCRIPTION OF EMBODIMENTS
FIG. 1 depicts an exemplary system 10 including an antenna having one or more antenna elements 12 that can be arranged in an array in horizontal (azimuth) and/or vertical (elevation) axes, as well as other configurations as desired. For example, the elements in the embodiment illustrated in FIG. 1 are arranged in arrays supported by a panel 14 , which are further connected via a frame 16 to form a deployable field unit. The system 10 includes at least one beam control element 20 that is positioned in accordance with the present invention and the application proximate the antenna 12 at a first angle, so as to attenuate radiation emitted from or approaching the antenna at angle greater than the first angle relative to radiation emitted from or approaching the antenna at angle less than the first angle.
It will be appreciated that the impact of the beam control element 20 can be described in terms of signals, or more generally radiation, passing through the antenna, or alternatively by the antenna performance, e.g., gain. For example, beam control element 20 can increase the antenna gain thereby enhancing the signal or radiation by increasing the intensity, total power in the main lobe, and/or the main lobe shape. Conversely, reducing the antenna gain produces attenuated signals/radiation. In addition, radiation and signals can be used interchangeably in various applications. Examples may focus on one description to facilitate the description of the invention, but unless otherwise noted are not intended to limit the invention.
The beam control element 20 can be implemented in a variety of systems 10 , such as radar systems including those described in U.S. Pat. No. 7,136,011, which is incorporated by reference, communication systems, etc. It should be noted that a beam control element 20 according to the invention may be part of a system 10 including a single antenna element, an array of elements, or even several arrays operating in an array of arrays. Unless otherwise noted, a reference to antenna element or array 12 hereinbelow is intended to cover any and all of these alternative configurations, and reference numeral 12 may refer to a single element or to a plurality of elements in an array or a plurality of arrays connected to the same transmitter.
Similarly, antenna will be used as a general term referring to any configuration of one or more antenna elements.
The beam control element 20 can include at least a partially reflective material positioned to reflect side lobe radiation in the direction of main lobe radiation. For example, the beam control element 20 can be configured to reflect and attenuate side lobe radiation emitted from the antenna at an angle that is greater than the first angle in the direction of main lobe radiation that is emitted from the antenna at an angle less than the first angle.
The beam control element 20 can be configured to attenuate to varying degrees signals, or radiation more generally, approaching and emitted from the antenna at an angle that is greater than the first angle. For example, if a reflective material is used, it can be configured to strongly reduce the signal power, or radiation intensity at the antenna at angles greater than the first angle by effectively reducing the antenna gain depending upon the amount of attenuating material used in combination with the reflective material. At the same time, the reflective material can be used to increase the antenna gain to enhance the radiation, i.e., increase the intensity or peak power, at angles less than the first angle to varying extents depending upon the amount of attenuating material used in combination with the reflective material.
In various embodiments, the beam control element 20 can be configured to minimize the impact on the antenna gain and the resulting signal or radiation characteristics at less than the first angle. For example, it may be desirable to limit the impact of the beam control element 20 on the main lobe, while modifying the side lobes. In other embodiments, it may be desirable to narrow or widen the main lobe, as well as control the maximum intensity of the signal/radiation or peak gain of the antenna.
Beam control element 20 can be positioned proximate one or more antenna depending upon the application. For example, the beam control element 20 can be symmetrically designed and positioned between two or more transmitter/receiver antenna elements, so as to impact the elements in a similar manner. In other embodiments or applications, asymmetric designs may be more useful depending upon the antenna design and position of the beam control element. In various embodiments, the beam control element 20 can be positioned proximate an antenna array at a first angle relative to the array and configured to reduce the antenna gain to attenuate signals approaching the array at an angle that is greater than the first angle and increase the antenna gain to enhance at least one signal emitted from the multiple antennas at an angle less than the first angle by reflecting radiation from angles greater than the first angle.
FIG. 2 shows a portion of a horizontal cross section of the system 10 of FIG. 1 , with vertical polarization-H plane is paper plane. A single antenna element 12 can include a ground plane 22 , the patch element 24 (electrical feed not shown), and a radome 26 . The radome 26 and the ground plane 22 may extend over several patch elements 24 . It will be obvious to a person skilled in the art that this beam control element is not limited to this array geometry, polarization and basic antenna element type, and is applicable for single or double sided use with any single element and/or array and basic antenna element type. The beam control element 20 can include a shielding plate 28 , absorber material 30 , and radome 26 . It will be appreciated that the radomes 26 may be integrated, as can ground planes 22 . In these exemplary embodiments, two elements 12 adjacent to each other in the horizontal direction have a nominal azimuth radiation reference axis between the two elements, and horizontally radiation may be steered close to 22.5 degrees from the axis by phase shifting signals to the two elements. If several elements are arranged adjacently in the vertical direction (perpendicular to the paper plane of FIG. 2 ), as shown in FIG. 1 , the radiation from the antenna may also be steered in the vertical direction.
The selection of the first angle can be influenced by a number of system design and operational objectives. For example, the first angle may depend upon the geometry of the system and the number of antenna elements being employed in each unit and the number of systems being deployed in a network. The design and material composition of the beam control element will generally be a consideration in the selection of the first angle.
FIG. 3 a depicts the main and side lobes of radiation being emitted from an antenna element 12 in the presence of an interfering object, such as a structure, 40 that could cause undesired reflections of the radiation back to the antenna. The first angle can be chosen relative to the main lobe axis of the antenna or antenna array to exclude the structure 40 from the radiation field of the antenna element or array 12 . It should be noted that in the absence of any steering of the main lobe axis by phase shifting, the main lobe axis of FIG. 3 a corresponds to the nominal azimuth radiation reference axis of FIG. 2 .
FIG. 3 b shows the placement of the beam control element 20 at the first angle, so as to strongly reduce the resultant gain of the antenna element 12 at angles towards the structure 40 . This configuration reduces the radiation into, as well as reflections from, the structure 40 . Whether the beam control element 20 reduces gain at all angles or a gives combination of reduced gain at angles greater than a given angle and increased gain at angles less than the same angle may depend on the magnitude of the first angle and the characteristics of the beam control element 20 . In the case of an interfering object 40 and the antenna used for radar application, transmission via object 40 may create separate mirror images of the observed object at false angles or the mirror image may mix with the direct radiated reflections from the observed object to reduce the angular accuracy of the radar.
Depending upon the system objectives, adversely impacting the radiation is attenuating the radiation to an extent that the system performance is degraded beyond operational requirements. In other words, the radiation emitted from the antenna at an angle less than the first angle can be modified without substantially diminishing it. In general, the first angle is selected such that the side lobes are attenuated as much as possible without adversely impacting the gain of the main lobe. In various embodiments, the beam control element configuration is balanced to enhance at least a portion of the radiation, i.e., main lobe, peak intensity, etc., while diminishing radiation in the side lobes. In other words, increasing the antenna gain relative to the main lobe, while reducing the antenna gain relative to the side lobes.
In various embodiments, the beam control element 20 is a layered combination of reflective and absorptive material. The reflective material being employed to substantially block the radiation, i.e., signals, approaching the antenna from angles greater than the first angle from reaching the antenna. The reflective material can also serve to reflect radiation emitted by the antenna at angles greater than the first angle in the direction of radiation emitted by the antenna at angles less than the first angle. The beam control element 20 can be configured such that reflected radiation emitted by the antenna could enhance the radiation level at angles less than the first angle. Exemplary reflective materials are generally materials that tend not to absorb significantly and to be opaque to radiation at the frequency of interest. For example, aluminum is an effective reflective material for radar applications. It will be appreciated that materials employed in various embodiments can range from partially reflective to fully reflective depending upon the application.
The absorptive material is provided to attenuate radiation approaching or emitted from the antenna at angles greater than the first angle. The amount of absorptive material used and its configuration in the beam control element depends upon the desirable beam shape of the radiation. For example, if a sharp beam shape for the main lobe of the radiation is desired or potential interference from reflected or nearby radiation sources may pose a problem, then the absorptive material would be increased accordingly. Conversely, if it is desirable to detect reflected radiation and there are not other nearby interference sources, then a lesser amount of absorptive material can be used. Exemplary absorber materials include commercially available RF absorber material, such as those sold by ETS-Lindgren and ECCOSORB® AN from Emerson & Cuming. The thickness/amount of absorber material will depend upon the frequency of interest and the desired amount of attenuation in the application. For example, in a radar application at 1.3 GHz, absorber thicknesses on the order of 25 mm can provide significant side and back lobe and wide angle attenuation, while still allowing main lobe beam sharpening via the reflective material.
The physical shape of the beam control elements can be varied depending upon the system requirements. For example, if the beam control element 20 is to be positioned between two antennas, then it may be desirable for the element to be symmetrically shaped, if a similar impact is desired for both antennas. If the element will be positioned with antennas on only one side, then each side of the element can be configured to achieve its specific objective. For example, the side of the element opposite the side of an antenna may best serve its intended function with a different shape and material. In planar beam control element 20 embodiments, the absorber material is layered on one or both sides of a reflective layer depending upon the application.
The beam control elements 20 can be located in various positions relative to the antenna element. In many applications, the beam control element 20 will be located only along a portion of the perimeter of the antenna. The beam control element 20 is particularly useful when there is a reflective body within the radiative or receiving range of the antenna or another antenna operating in a manner that would interfere with the proper function of the system. The beam control element 20 is positioned along the perimeter of the antenna element at a first angle such that reflections of radiation from the reflective body are not received or radiation is not transmitted to or received from a source/sink to be excluded. While beam control elements 20 could be deployed around the entire perimeter of the antenna, it would increase the cost of the system without necessarily providing an associated benefit. In fact, it may be desirable to not include beam control elements 20 except along specific portions of the perimeter, because the beam control element could limit the performance of the antenna in portions where they are not necessary.
In many instances, it is desirable to have a system that provides 360 degree coverage area. However, in some applications it may be desirable to eliminate antennas from the system that point generally toward a known reflective body or another system that could interfere with the performance of the system. Elimination of the antennas 12 pointing toward reflective bodies can improve the overall system performance, because secondary reflections from the known body that reach other antennas are eliminated.
In many applications, the beam control elements will only be deployed along the perimeter of the antenna elements where there is a known reflective body 40 that could interfere with the performance of the system, such as the detection of targets within the coverage area of a radar. In an exemplary radar application, the radar is placed in close proximity to a tower, or other obstacle, to detect targets that are approaching the tower. In these examples, it may be desirable to not place antennas in locations where the antennas 12 would emit radiation directly toward the tower 40 . Beam control elements 12 would be deployed proximate antennas that might otherwise receive radiation directly reflected from the tower 40 , as in FIG. 8 b discussed below.
In many embodiments, the beam control element will be electrically decoupled from the antenna, so its impact is on the radiation. In other embodiments, it may be beneficial to couple the antenna and the beam control element to achieve an operational objective. Also, the beam control element 20 can be placed between antenna 12 to minimize and possibly eliminate mutual coupling of the antenna 12 .
FIG. 4 shows a 2×8 array from the back side with the Z axis being the reference azimuth beam angle used for verification. It will be obvious to a person skilled in the art that the invention is not limited to this specific array or type of antenna element, and not limited to this specific geometry.
FIG. 5 shows the antenna gain as a function of azimuth angle with and without the beam control element 20 . No phase steering is applied and the beam is pointed in z axis from FIGS. 2 and 4 . Overlaid on the graph showing the data without the beam control element 20 (dotted line) are lines showing the approximate demarcation of the main lobe and side lobes. As can be seen in the graph, from the angle of the beam control element, which in this example is positioned at −22.5 degrees, the added attenuation is approx. 4 dB (one-way), rising to 13 dB at −45 degrees, 22.5 degrees beyond the beam control element 20 . As also seen, the side lobe is attenuated by 16 dB at −70 degrees. Tests results shown are at 1325 MHz, but similar results apply from 1307 to 1342 MHz. In addition, the beam control element enhances the maximum gain in the main lobe relative to operation without the beam control element. As can be seen, the beam control element 20 , while not completely eliminating the side lobes, does substantially block the side lobes attenuating the signals, or reducing the antenna gain, in excess of 90%.
FIG. 6 shows results using an azimuth beam with one beam control element 20 positioned at −22.5 degrees relative to the nominal azimuth radiation reference axis and for various steered angles. FIG. 6 also shows antenna gain when the beam is steered towards and away from the beam control element. Side lobes are completely attenuated when steering the beam towards the beam control element. Side lobes reappear when steering away from the beam control element, but is attenuated compared to the corresponding side lobes without the beam control element.
FIG. 7 shows that the elevation (perpendicular, E field axis, Azimuth beam at 0 degrees, elevation beam steered) is almost unaffected by the beam control element, when deployed in an array.
While the beam control element can be configured in many ways in the present invention, it is often desirable to have a number of the following properties:
Preferably passive, such as a combination of absorbing and reflective (shielding) materials. Simple mechanical construction of sandwich for low cost manufacturing. Positioned in the antenna near field where a small size, weight and cost is possible rather than covering larger structures with absorbers or reflective elements Positioned outside the antenna main lobe, for minimum main lobe loss and attenuation of desired signals and inside the antenna side lobe, maximising the side and back lobe attenuation. Suitable for reduction and practical radiation cut-off towards external structures that would otherwise block or distort signal and create undesired reflections and to reduce antenna radiation to near zero at a well defined radiation angle. Robust to various steered main beam angles in a phased array antenna, where the lobe may be steered both in the axis of the absorber element and in the perpendicular axis or only one of the said axes. The distortion of the beam in the perpendicular axis is negligible. The distortion of the beam in the axis of the beam control element is well controlled even when the main beam is steered close to the angle of the beam control element. Predictable effect on the antenna beam, which may predictably be compensated in subsequent signal processing, i.e., good correspondence between 3D electromagnetic simulation and measurements. Well controlled and predictable radiation patterns even with beam steering in both axes allow high accuracy radar performance even at scan angles close to a physical structure where accuracy would otherwise be compromised when using low gain antennas. Allows operation at scan angles close to undesired objects as towers and buildings, insensitive to changes in the undesired object to be masked. Increases the effective main lobe gain towards the side of the beam control element. The increased gain is comparable to using a higher order antenna array. As example, an array of 2 with the beam control element performs comparable to an array of 4 elements at the side of the lobe control element.
In various embodiments, the beam control elements are configured to allow two or more antennas to have overlapping coverage areas, while still performing the task of attenuating and enhancing the various signals. In other embodiments, the beam control elements will be configured to minimize or eliminate overlap between antenna coverage areas. The skilled artisan will appreciate the trade-offs with overlapping providing a continuous coverage area and non-overlapping allowing the reuse of spectrum, etc. for multiple antenna. For example, in radar applications it may be desirable to provide overlapping coverage area to ensure that targets that are being detected by the radar can be continuously tracked within the coverage area. In communications application, it may not be desirable to have overlapping ranges, if the same frequency spectrum is going to be used.
The present invention can be employed in a number of applications including radar antennas, cellular network base station antennas, limiting undesired (culprit) antenna side lobe radiation for various technical reasons or public health reasons, reducing interference sensitivity from the side lobes of the (victim) antenna, etc.
FIGS. 8 a & b show embodiments (not necessarily to scale) of the system 10 deployed proximate the structure 40 . In these embodiments, antenna elements 12 can be provided azimuthally and/or vertically to provide a substantially continuous coverage area in the azimuthal plane. It will be appreciated that antenna elements will usually not be deployed in the direction of the structure(s) 40 to reduce cost and/or control performance. In the present invention, one or more beam control elements 20 can be deployed to prevent reflections from the structure 40 from being received by the antenna elements 12 . While FIG. 8 a & b shows only one structure 40 , it will be appreciated that many structures 40 can be in a potential coverage area for the system 10 , such as in a windmill park, and the azimuthal coverage angle of the system 10 and the number and design of beam control elements 20 can be varied to accommodate the particular deployment.
In radar antenna embodiments, the system 10 may be installed at towers and buildings where these structures 40 will partially block the angle of view, and may generate undesired signal paths that reduce radar angle measurement accuracy, as described above. The beam control element 20 assures a predictable cutoff of radiation into the external structure 40 , allowing good accuracy at steered beam azimuth angles less than 5 degrees from the beam control element. In these embodiments, it may be desirable to provide less than 360 coverage due to the proximity of the physical structure 40 . As such, not only will beam control element 20 be used to substantially block radiation from being transmitted toward or reflected by the structure 40 , but the system 10 can be configured to exclude antenna elements 12 or scans in the direction of the physical structure 40 , as shown in the figures.
FIG. 9 a depicts communication tower embodiments, such as for cellular network base station antennas and other wireless communication systems, in which multiple systems 10 are positioned proximate the structure 40 . The basic antennas are normally arrays with high elevation gain and low azimuth gain, where the azimuth side and back lobes may radiate well into neighbour and next-neighbour cells such that these cells must be separated in frequency, code or time to prevent interference. In these applications, the beam control element 12 can improve the isolation between each cell in the azimuth axis, allowing increased re-use of frequency, code or time slots at the base station, in addition to preventing interference from the structure. Reuse in communication applications can provide a significant benefit in that reuse effectively increases the available bandwidth of the station.
FIG. 9 b depicts embodiments of the invention, in which the system 10 can be used as a gap filler, or shadow, radar system for use in areas where a primary radar 50 can not provide adequate coverage of the area for any number of reasons including the presence of structures, e.g., buildings, and restrictions on the use of radar near installations and facilities. In these embodiments, the beam control element would help decrease reflections from the primary radar that reach the antenna 12 . One of ordinary skill will appreciate that the system 10 and radar 50 may need to operate at different frequencies and orientations to ensure the effectiveness of the system 10 in providing radar coverage in areas not adequately covered by the primary radar 50 .
FIG. 10 shows embodiment in which the antenna elements 12 of the system 10 are deployed surrounding and/or integrated with the one of the structures 40 . While FIG. 10 embodiments show antenna elements 12 deployed only partly around the perimeter of the structure 40 and in combination with beam control elements, it will be appreciated that number and angular extent of antenna elements 12 and beam control elements 20 positioned around the structure 40 can be varied by the skilled artisan to specific deployments and applications. It will be further appreciated that other parts of the system 10 , which could include central processing units, communication equipment, etc. can be deployed proximate the antenna elements 12 on the structure 40 or not proximate to the antenna elements 12 , for example on the ground or proximate another access point to the structure 40 .
These and other variations, modifications, and applications of the present invention are possible and contemplated, and it is intended that the foregoing specification and the following claims cover such variations, modifications, and applications. | The present invention provides, among other things, antenna beam control devices, systems, architectures, and methods for radar and other applications, such as wireless communications, etc., to improve transmit and/or receive performance of the devices and systems employing such antennas by deploying beam control elements ( 20 ) to increase antenna gain at an angle less than a first angle relative to the antenna gain at angle greater than a first angle. Beam control elements are deployed in combination with the one or more antennas ( 12 ) in various systems of the present invention, such that the impact of reflected radiation from wind mill, communication, or other towers supporting the system or other nearby structures, as well as radiation from nearby wireless communication networks is decreased to an acceptable level. The beam control elements can include absorbing and reflective material and can be placed in the antenna near field to minimize costs. | 7 |
RELATION TO PRIOR APPLICATIONS
[0001] This application claims priority 35 U.S.C. § 119(e) to U.S. Provisional Application No. 60/689,806, filed Jun. 13, 2005.
FIELD OF THE INVENTION
[0002] The invention relates to methods and kits for diagnosing and treating cerebrovascular events, and for defining the time and anatomical location of an event, based on the detection and quantification of bound or total and unbound NR2 peptides in biological fluids. The methods are optionally performed in conjunction with neurological scoring and neuroimaging, and directed to risk assessment, prognosis, diagnosis and treatment of TIA and stroke on an emergency basis in the emergency room and in a primary care setting.
BACKGROUND OF THE INVENTION
Cerebrovascular Accident and Transient Ischemic Attack
[0003] Transient ischemic attack portends significant future risk of stroke and its associated morbidity and mortality. Patients with transient ischemic attack require further evaluation to assess for any potentially reversible underlying disease process. Despite the significant impact of this disease process there is still no definitive guidance concerning the early evaluation and disposition of such patients presenting to the Emergency Department. The Stroke Council of the American Heart Association states there is no prospective data concerning the justification for inpatient evaluation of patients with TIA. They conclude that “the decision whether to hospitalize a patient depends on that patients individual circumstances.” Considerable regional practice variation exists in the initial evaluation of such patients on an inpatient versus outpatient basis. The rationale for inpatient care is to expeditiously obtain diagnostic studies, evaluate risks for future events, monitor the patient for recurrence or worsening symptoms, and to institute any needed interventions including operative therapy. Current recommendations for the evaluation and treatment of patients with TIA are well described. The guidelines suggest a battery of laboratory tests and radiologic studies along with recommendations concerning medical and surgical therapy.
[0004] It appears that a certain subset of patients presenting to the Emergency Department with symptoms suggestive of TIA are at substantial risk in the short term of suffering a completed stroke. In a recent Emergency Department-based observational cohort study involving 1707 patients presenting with symptoms suggestive of TIA, 10.5% of patients developed stroke within 90 days. Significantly, half of those patients developed a stroke within the first 2 days. Johnston et al retrospectively identified five independent risk factors for stroke within 90 days (age>60, Diabetes, Duration of symptoms >10 min., Weakness, Speech impairment). By combining the independent risk factors, subgroups were identified with minimal (0%) to high (34%) short-term risk of stroke.
[0005] Such high-risk patients are unlikely to receive a complete diagnostic evaluation and implementation of an appropriate therapeutic regimen (medical or surgical) as an outpatient in less than 48 hours. Further complicating the decision process is the degree of diagnostic certainty in patients with a suspected TIA. Transient ischemic attack is a clinical diagnosis and inter-observer reliability concerning the diagnosis is often poor. Therefore, in the setting of current practice patterns in many institutions, some patients without true neurologic disease are admitted as well as others who may fare just as well with an outpatient evaluation. Prospective validation of a set of risk factors identifying patients who complete stroke within days of a sentinel TIA would allow for the derivation of a clinical prediction rule. This would allow for identification of patients at high risk in the near term that require admission as well as those who may be safely discharged for an outpatient evaluation. Such “stratification of stroke risk” would allow targeting of more aggressive interventions to those at greatest short-term risk.
Current Alternatives to Stroke Diagnosis
[0006] The medical community has several technologies to diagnose stroke. Although numerous, none of these technologies is able to predict stroke or directly diagnose cerebrovascular abnormalities or TIA/stroke. In the stroke treatment field, the adage all physicians live by are “Time is Brain”.
[0007] The National Institute of Neurological Disorders and Stroke (NINDS) recommends the following time guidelines for managing ischemic stroke:
[0000]
Door to physician
10
min
Door to neurologic consultation
15
min
Door to CT completion/interpretation
45
min
Door to thrombolytic treatment
60
min
Door to neurosurgical consultation
2
hr
[0008] Emergency Departments at major hospitals have a wide range of options for diagnosing stroke. More than 90% of hospitals with more than 200 beds have access to CT scanners, enabling them to quickly (<15 min) evaluate a potential stroke patient to rule out hemorrhagic stroke and stroke mimics. It is theoretically possible for CT to positively identify 100% of parenchymal and 85 to 97% of subarachnoid hemorrhages, however overall accuracy of recognition of ischemic vs. hemorrhagic falls with interpretation to between 67 and 83 percent.
[0009] A large percentage of hospitals now have Magnetic Resonance Imaging (MRI) capability. However, MRI scans require a longer time window for imaging. Currently MRI does not readily distinguish hemorrhagic stroke prior to 6 hrs and is thus not considered a primary diagnostic modality. A relatively new technology, Diffusion-Weighted Magnetic Resonance Imaging (DWI) can rapidly detect perfusion decreases in patients with high risk of TIA. Initial data found DWI predictive within less than 10 minutes of ischemic change. Scanning sequences can be obtained in 30 to 60 seconds of scanner time. Although effective, each of these imaging techniques is limited by high capital costs and service requirements. Furthermore, they require specially trained technicians to operate and interpret the results.
[0010] Other technologies, including Doppler Ultrasound, Single-Photon Emission Computerized Tomography, Xenon-Computerized Tomography, CT Angiography, and MR Perfusion Imaging have been omitted either for lack of a global diagnostic approach or the early stage of the current technology.
[0011] There are no blood tests currently available in the Emergency Department that answer these unmet diagnostic needs by diagnosing acute cerebrovascular accidents, TIA, and ischemic stroke and ruling out stroke mimics.
Brain NR2 Peptide and Antibody as Biomarkers of TIA/stroke
[0012] The majority of studies involving markers of the central nervous system come from brain injury or cardiothoracic literature. However the most significant marker for brain ischemia is NMDA receptors that are involved in the neurotoxicity cascade underlying cerebral ischemia.
[0013] Excitatory amino acids (EAAs) play an important role during stroke. Cerebral ischemia induces glutamate release, and activates EAA receptors. Blocking glutamate release or its interaction with EAA receptors has been reported to reduces cerebral damage. N-methyl-D-aspartate receptors (NMDAR), a member of the ligand-gated ion EAA channel complex, contain NR1, NR2 and NR3 subunits. Of these subunits, NR2 has been reported to be involved in several neurological disorders, including ischemia and hypoxia. The NR2 subunit consists of 4 different subtypes, NR2A-2D, which are encoded by different genes. Both NR2A and NR2B are found in the cerebral cortex and hippocampus whereas NR1 is ubiquitous to all NMDAR complexes located in brain and peripheral organs.
[0014] Over-stimulation of glutamate receptors during ischemia induces excessive Ca 2+ influx and activation of thrombin-activated serine proteases, which facilitates the cleavage of external N-terminal domain of NMDAR on cell membranes. The N-terminal peptide fragments of NMDAR, translocated to the bloodstream through the damaged blood-brain barrier, can possibly act as “foreign” antigens and initiate an immune response that generates antibodies in the blood. However the interaction between time course of NR2 peptide/antibodies in blood and NR2 mRNA expression in brain remains unclear.
[0015] Recently, NMDAR peptides and their antibodies have been proposed for the treatment of stroke and epilepsy (During et al, Science, 2000, 287:1453-60) and as biomarkers of neurotoxicity underlying cerebral ischemia and stroke (Dambinova S A, et al. Stroke 2002; 33:1181-1182; Dambinova S A, et al. Clin Chem 2003; 49:1752-1762). With neuronal death or ischemia, NR2 peptide fragments of the NMDA receptor break off and appear in the bloodstream and generate an antibody response. Dambinova et al. have reported that the peptide fragments and antibodies can both be detected in blood samples (Dambinova SA, et al. Stroke 2002). They have further reported that adult patients who have suffered an acute ischemic stroke have elevated blood levels of NR2 peptide/Ab that correlate with the amount of brain damage revealed through brain scans (MRI) and neurocognitive testing (Dambinova SA, et al. Clin Chem 2003; 49:1752-1762).
[0016] NR2 peptides and antibodies may have diagnostic as well as prognostic utility in the acute management of patients with cerebrovascular accidents, TIA and stroke. The evaluation of the presence or absence of such markers in the acute setting may improve diagnostic/prognostic accuracy as well as define those patients at increased risk for subsequent stroke.
OBJECTS OF THE INVENTION
[0017] The medical community faces several principal diagnostic challenges in overall stroke management, including differentiating brain ischemic attack from hemorrhage and stroke like disorders, and evaluating the risk of stroke or other complicating factors. In the present invention, blood assays for detecting bound or total and unbound NR2 peptide were developed, and used to differentiate cerebrovascular accidents such as TIA and stroke from cerebral hemorrhage and stroke mimics.
[0018] Therefore, it is an object of the invention to unbound NR2 peptide test to evaluate acute cerebrovascular accidents and TIA/stroke as defined by DWI/MRI for better diagnosis, management and treatment.
[0019] It is another object of the present invention to detect bound or total NR2 peptide to accurately diagnose chronic TIA and stroke to the exclusion of stroke-like disorders in conjunction with NIHSS evaluations and neuroimaging.
[0020] It is still another object of the present invention to distinguish between new and old brain lesion areas and lacunar strokes defined by DWI, by measuring for increased concentrations of bound or total and unbound NR2 peptides above population norms.
[0021] Still another object of the invention is to help predict the likely occurrence of a subsequent cerebrovascular accident leading to progression to completed stroke based on concentrations of unbound and bound or total NR2 peptide.
[0022] Still another object of the invention is to help evaluate the severity of symptoms suggestive of potential TIA depending on concentrations of unbound and bound or total NR2 peptide.
[0023] It is another object of the present invention to evaluate infarction size based on DWI/MRI and concentrations/ratios of unbound and bound or total NR2 peptide.
[0024] It is another object of the present invention is to provide methods for real-time assessments of NR2 peptides and antibodies and ratios, and for determining therapeutic windows in patients with cerebrovascular accidents or TIA/stroke for timely neuroprotective therapy.
[0025] Still another object of the present invention is to provide diagnostic tests for detecting unbound and bound or total NR2 peptide as additional tools to neurological observations and neuroimaging in identifying patients who are at subsequently high risk in the near term of completed stroke.
SUMMARY OF THE INVENTION
[0026] It has been unexpectedly discovered that levels of circulating NR2 peptides that are bound to immunoglobulins, albumin and other peptide carriers in the blood (hereinafter “bound NR2 peptides”), which are not detected in conventional NR2 test kits or testing regimens, provide useful diagnostic information to clinicians evaluating TIA and stroke and stroke-like disorders and brain damage underlying these cerebrovascular events. The detection and quantification of these bound NR2 peptides can be used to diagnose the existence of brain lesions resulting from insufficient blood circulation or microembolic events, and can greatly increase the accuracy of diagnoses and subsequent treatment efficacy, especially when used in combination with other diagnostic tests such as tests for unbound NR2 peptides, NIHSS scoring and neuroimaging.
[0027] The rapid evaluation of these brain markers in emergency room settings will greatly enhance the physicians' ability to identify patients who are suffering an acute cerebrovascular event such as TIA or stroke, and help physicians determine whether a cerebrovascular event is an ischemic event, a hemorrhagic stroke or a stroke-like disorder. In emergency rooms and every doctor's office, the use of the brain markers will help identify patients at risk for having an ischemic stroke, and assist in the development of neuroprotective regimens.
[0028] It has been determined experimentally that total NR2 peptide concentrations greater than about 2.0 ng/ml (i.e. bound and unbound peptides) are above the norm for healthy individuals, and portend an unhealthy cerebrovascular state, especially when combined with a level of unbound NR2 peptides above the norm for healthy individuals (i.e. greater than about 0.5-0.6 ng/ml). When evaluating a patient suffering from a neurological deficit, a comparison of concentrations of total and unbound peptide concentrations has remarkable diagnostic capacity to determine whether the underlying ischemic is a recurrent episode or flare-up of a chronic condition, or whether the patient is experiencing a primary cerebrovascular accident. In particular, the combination of (1) a total peptide concentration greater than about 2.0 ng./ml. and (2) a total:unbound peptide ratio greater than about 2:1 correlates well with a recurrent event, especially when combined with an unbound peptide concentration less than about 2.0, 1.0, 0.8, 0.6 or 0.5 ng/ml. In contrast, a combination of (1) an unbound peptide concentration greater than about 1.0 ng./ml. and a total:unbound peptide ratio less than about 2:1, correlates well with a primary event, especially when combined with a total peptide concentration less than about 3.0 or 2.0 ng./ml.
[0029] Once again, these correlations can be extensively used for the choice of emergency treatment such as anti-platelet or neuroprotective therapy in a short time frame. The biomarker profile provides real time evidence of a cerebrovascular accident, and the reduction in concentration of circulating total NR2 peptide correlates well with positive effect of chosen therapy. The methods of the present invention also can be employed in a primary care setting, when evaluating a cerebrovascular accident or TIA, and in identifying patients who are at subsequently high risk in the near term of TIA or completed stroke. In addition, based upon results showing an increased risk of suffering TIA or stroke, prevention therapy can be administered, and the effectiveness of the therapy monitored using the methods of the present invention.
[0030] Additional advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The advantages of the invention will be realized and attained by means of the elements and combinations particularly pointed out in the appended claims. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
DESCRIPTION OF THE DRAWINGS
[0031] The accompanying drawing, which are incorporated in and constitute a part of this specification, illustrate several embodiments of the invention and together with the description, serve to explain the principles of the invention.
[0032] FIG. 1 is a graphical depiction of the distribution of unbound NR2 peptide in plasma of patients studied (n=40) in the examples of the present invention.
[0033] FIG. 2 is a graphical depiction of the distribution of total NR2 peptide in plasma of patients studied (n=40) in the examples of the present invention.
[0034] FIG. 3 is a flow chart diagramming the proposed standard of care for patients presenting with symptoms of TIA and/or stroke in an emergency room setting.
[0035] FIG. 4 is a diagram of the various factors and neurological deficits that are addressed when diagnosing stroke incidence and severity using the National Institutes of Health Stroke Scale (“NIHSS”).
DETAILED DESCRIPTION OF THE INVENTION
[0036] The present invention may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the Examples included therein.
DEFINITIONS AND USE OF TERMS
[0037] As used in this specification and in the claims which follow, the singular forms “a,” “an” and “the” include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to “a fragment” includes mixtures of fragments, reference to “an cDNA oligonucleotide” includes more than one oligonucleotide, and the like.
[0038] “Polypeptide,” “protein” and “peptide” are used interchangeably herein and include a molecular chain of amino acids linked through peptide bonds. The terms do not refer to a specific length of the product. Thus, “peptides,” “oligopeptides,” and “proteins” are included within the definition of polypeptide. The terms include post-translational modifications (isoforms) of the polypeptide, for example, glycosylations, acetylations, phosphorylations, chelates, and the like. In addition, protein fragments, analogs, mutated or variant proteins, chimeric peptides and the like are included within the meaning of polypeptide. The polypeptide, protein and peptides may be in cyclic form or they may be in linear form.
[0039] An NMDA receptor or NMDAR is one of a family of ligand-gated ion channels that bind preferentially to N-methyl-D-aspartate and that mediate the vast majority of excitatory neurotransmission in the brain (Dingledine R. et al., Pharmacol Rev. 1999 March; 51(1):7-61.). The receptors include subunits reported in the literature as NR1, NR2A, NR2B, NR2C, NR2D, NR3A and NR3B, that perform distinct pharmacological functions. GenEMBL Accession Nos. have been reported for NR1 (X58633), NR2A (U09002) and NR2B (U28861), and are described in WO 02/12892 to Dambinova.
[0040] An NMDA receptor peptide refers to a full length NMDA receptor protein, a peptide fragment of the naturally or synthetically occurring full length NMDA receptor, or an anologue or isoform thereof. An NR2 peptide thus includes the full length NR2A, NR2B, NR2C and NR2D subunits, in addition to fragments, analogs and derivatives thereof. Similarly, an NR2A, NR2B, NR2C, or NR2D peptide means the full length naturally occurring NR2A, NR2B, NR2C or NR2D peptide subunits, or a fragment, analog or derivative thereof. The N-terminal domain of NMDA peptides refers to the amino acid N-terminal domain fragment of the full length peptide, or a fragment, analog or derivative thereof, typically about 40 or 50 amino acids long, but as much as 150, 200 or 300 amino acids long, as described in WO 02/12892 to Dambinova.
[0041] An “analogue” of a peptide means a peptide that contains one or more amino acid substitutions, deletions, additions, or rearrangements. For example, it is well known in the art of protein biochemistry that an amino acid belonging to a grouping of amino acids having a particular size or characteristic (such as charge, hydrophobicity, and hydrophilicity) can often be substituted for another amino acid without altering the activity of the protein, particularly in regions of the protein that are not directly associated with biological activity. Thus, an analogue of an NMDA peptide is useful in the present invention if it includes amino acid substitutions, deletions, additions or rearrangements at sites such that antibodies raised against the analogue are still specific against the NMDAR peptide.
[0042] Unless stated to the contrary, an NMDAR analogue or mutant as used in this document refers to a sequence that has at least 80% amino acid identity with naturally occurring NMDA, although it could also contain at least 85%, 90%, or 95% identity. Amino acid identity is defined by an analogue comparison between the analogue or mutant and naturally occurring NMDA. The two amino acid sequences are aligned in such a way that maximizes the number of amino acids in common along the length of their sequences; gaps in either or both sequences are permitted in making the alignment in order to maximize the number of common amino acids. The percentage amino acid identity is the higher of the following two numbers: (1) the number of amino acids that the two peptides have in common with the alignment, divided by the number of amino acids in the NMDA analogue, multiplied by 100, or (2) the number of amino acids that the two peptides have in common with the alignment, divided by the number of amino acids in naturally occurring NMDA peptide, multiplied by 100. Amino acids appended to the ends of the fragment under analysis are not taken into consideration.
[0043] NMDA derivatives include naturally occurring NMDA and NMDA analogues and fragments thereof that are chemically or enzymatically derivatized at one or more constituent amino acids, including side chain modifications, backbone modifications, and N- and C-terminal modifications, by for example acetylation, hydroxylation, methylation, amidation, phosphorylation or glycosylation. The term also includes NMDA salts such as zinc NMDA and ammonium NMDA.
[0044] The term “antibody” is synonymous with “immunoglobulin.” As used herein, the term “antibody” includes both the native antibody, monoclonally generated antibodies, polyclonally generated antibodies, recombinant DNA antibodies, and biologically active derivatives of antibodies, such as, for example, Fab′, F(ab′) 2 or Fv as well as single-domains and single-chain antibodies. A biologically active derivative of an antibody is included within this definition as long as it retains the ability to bind the specified antigen. Thus, an NR2 antibody that binds specifically to an NR2 peptide has the ability to bind at least one NR2 peptide.
[0045] The term “NR2” peptide refers to any peptide expressed in the NR2 subfamily of NMDA receptors, including full length NR2A, NR2B, NR2C and NR2D subunits, fragments thereof, and recombined fragments thereof. A preferred NR2 peptide for practicing the present invention is recombined from sequences within the NR2A and NR2B subunits, or analogs thereof. The sequences are preferably autoantigenic, and preferably derive from the N-terminal domain of the recited NMDA receptor subtype. The peptides are preferably less than about 40 amino acids in length, and greater than about 15 amino acids. It will of course be understood that analogs of such sequences may also be present in the recombinant peptide.
[0046] A preferred NR2 peptide is a recombinant NR2A/NR2B peptide, and has the following nucleotide sequence:
NGMIGEVVYQRAVMAVGSLTIKRIVTEKTD 31
[0048] A “protein detergent” refers to any compound capable of freeing NR2 peptides from circulating complexes in the human blood stream, including various ionic surfactants and amphiphilic molecules that are generally known in the art. Examples include sodium dodecyl sulfate (a/k/a sodium lauryl sulfate), sodium taurocholate, sodium cholate, CTAB, LDAO, CHAPS, Tween 20, Thesit, Triton X-100, NP40, n-octyl sucrose, n-dodecyl sucrose, n-dodecyl maltoside, octyl glucoside, octyl thioglucoside, n-hexyl glucoside and n-dodecyl glucoside.
General Discussion
[0049] The present disclosure describes diagnostic and therapeutic applications that result from the realization that genetic or accidental increase of NMDA receptors synthesis in the brain reflects a neurological ischemic deficit, and may be used for fast diagnosis of stroke or TIA and to distinguish from other stroke-like disorders. NMDA receptors that are abnormally expressed in the brain are quickly metabolized and, following penetration of the blood brain barrier, these metabolic destruction products enter the circulatory system. The immune system recognizes these peptides and protein fragments as foreign antigens and responds by generating antibodies and immune complexes. Once bound in these immune complexes, and other agglomerates such as albumin complexes in the bloodstream, these peptides are largely unavailable for detection in conventional testing regimens. In the present invention the content of bound NR2 peptide (bound antigen) or total NR2 peptide, and optionally unbound NR2 peptide (free antigen), are evaluated as brain biomarkers for their prognostic/diagnostic value when evaluating cerebrovascular accidents, TIA and stroke, and the risk of future cerebrovascular accidents, TIA and stroke.
[0050] Thus, in one aspect the present invention provides a method for diagnosing a central nervous system disorder comprising measuring amounts of bound or total NR2 peptide or NMDA receptors fragments in a biological sample, and optionally measuring unbound NR2 peptide. In another embodiment, the invention provides A method for determining the pathological origin of a neurological deficit comprising: (a) providing a patient suffering from a neurological deficit; (b) detecting and quantifying bound or total NR2 peptide in a biological fluid from said patient to arrive at a quantity of bound or total NR2 peptide; and (c) comparing said quantity of bound or total NR2 peptide with a population norm for bound or total NR2 peptide in said biological fluid in apparently healthy human subjects. In a particularly preferred embodiment, the method further comprises: (a) detecting and quantifying unbound NR2 peptide in a biological fluid from said patient to arrive at a quantity of unbound NR2 peptide; and (b) comparing said quantity of unbound NR2 peptide with a population norm for unbound NR2 peptide in said biological fluid in apparently healthy human subjects.
[0051] Elevated levels of NR2 peptide are specific to brain damage, and are expressed in ischemic brain tissue at higher rates than other NMDA receptors, and thus are uniquely suited for assessing cerebral ischemic episodes, TIA and stroke. Baseline levels for determining whether the measured concentrations of unbound and bound or total NR2 peptide are elevated, and hence indicative of a central nervous system disorder, can be obtained from population norms or, preferably, from a patient's own test history.
[0052] Immunoassay techniques are generally preferred for measuring the proteins or peptides of the present invention, although other analytical techniques are also available as known to those skilled in the art, such as HPLC. However, when using immunoassays it has been found that the antigenic determinants are concentrated in the N-terminal domain of the NR2 type of NMDA receptor, and that antibodies rose against the N-terminal domains and fragments thereof should be employed for optimal test results.
[0053] The methods of the present invention are preferably performed by directly measuring the concentrations of unbound and bound or total NR2 peptides in a selected biological sample, using immunoassay techniques employing antibodies raised against the biomarkers by direct ELISA, or through quantitative techniques such as HPLC. If unbound and bound or total NR2 peptides are measured, they are preferably measured using one or more antigenic fragments of the NR2 peptide as the target of the antibody, as opposed to a whole NR2 type of NMDA receptor. Healthy persons generally have unbound NR2 peptide blood concentrations less than about 2.0, 1.0, 0.8, 0.6 or 0.5 ng/ml and total NR2 peptide blood concentrations less than about 3.0, 2.0 or 1.5 ng/ml.
[0054] The methods of the present invention can be performed using practically any biological fluid where circulating cerebral NMDA receptors, or markers of such receptors, are expressed or found, including blood, urine, blood plasma, blood serum, cerebrospinal fluid, saliva, perspiration or brain tissue. In a preferred embodiment the biological fluid is plasma or serum, and in an even more preferred embodiment the plasma or serum is diluted to a ratio of about 1:50.
Emergency Room Diagnosis and Rehabilitation Prognosis
[0055] As mentioned above, the methods of the present invention are especially well suited for use in emergency room setting because NR2 peptide or NMDA receptor fragments levels are elevated at a very fast and early stage of ischemic events and thus provide a real time indication of brain damage especially when measured in conjunction with NIHSS and CT or DWI//MRI. In a preferred embodiment, the patient is evaluated while the ischemic event is ongoing, preferably in time to intervene with neuroprotective therapy. Thus, for example, the patient may be evaluated while experiencing a neurological deficit. Alternatively, the patient may be evaluated within about 6, 5, 4, 3, 2 or even fewer hours after initial onset of stroke-like symptoms. Therefore, in one embodiment the invention provides a method for evaluating brain status by blood tests, or the existence of a central nervous system disorder such as cerebrovascular accident, TIA or stroke, by withdrawing the biological sample from a human within three hours of the onset of stroke-like symptoms.
[0056] The methods of the present invention are also especially useful in an emergency room setting when adapted to a latex agglutination assay, because of the speed and ease with which the latex agglutination procedure can be employed. Using the latex agglutination processes bedside, a care provider can often obtain blood test results in less than 10 minutes. Thus, using the methods of the present invention real-time data can be obtained even in the “field” during patient transportation, that will offer a greater window of time for neuroprotective treatment. Therefore in still another embodiment of the invention, the amount of time elapsed between withdrawing the biological sample from the subject, and detecting or measuring the presence or quantity of unbound and bound or total NR2 peptide or NMDA receptor fragments, is less than 30 minutes.
[0057] One of the most pronounced advantages of the present invention is the ability to distinguish ischemic episodes such as stroke from other stroke-like disorders such as brain tumor, traumatic brain injury, abscess, air embolism, giant cell arteritis, collagen vascular diseases, metabolic abnormalities, Bell's palsy, labyrinthitis, or demyelinating diseases. This advantage is available regardless of whether the peptide detected is bound or unbound, and this aspect of the invention applies to regardless of whether the peptide detected is bound or unbound, or whether both peptides are detected. In particular, if a stroke is suspected, the method will help diagnose whether the stroke is an ischemic or hemorrhagic insult, and guide the practitioner toward a neuroprotective therapy that is suited to the type of stroke diagnosed. Thus, in another embodiment the invention provides a method for diagnosing the existence of a cerebrovascular disorder, TIA or stroke further comprising, when the diagnosis confirms a stroke, evaluating from concentrations of unbound and/or bound or total NR2 peptide or NMDA receptor fragments whether the stroke is ischemic or hemorrhagic and administering ischemic or hemorrhagic stroke therapy as appropriate.
[0058] In one embodiment the therapy under consideration is tissue plasminogen activator (tPA), and the invention provides a method of diagnosing and treating cerebral ischemia comprising: (a) providing a patient suffering from a neurological deficit; (b) detecting and quantifying NR2 peptide (bound and/or unbound) in a biological fluid from said patient to obtain a first quantity of NR2 peptide; (c) comparing said first quantity of NR2 peptide with a population norm for NR2 peptide in said biological fluid in apparently healthy human subjects; (d) administering tPA to said patient if said first quantity of said NR2 peptide is above the population norm for NR2 peptide in said biological fluid in apparently healthy human subjects; and (e) not administering tPA to said patient if said quantity of said NR2 peptide is below the population norm for NR2 peptide in said biological fluid in apparently healthy human subjects. In a preferred embodiment, bound or total and unbound NR2 peptide are separately detected and quantified to arrive at quantities of bound or total and unbound NR2 peptides, and said quantities of said bound or total and unbound NR2 peptide are compared with population norms of bound or total and unbound NR2 peptides in said biological fluid in apparently healthy human subjects.
[0059] In another embodiment, the method is performed by (a) evaluating said patient for acute facial paresis, arm drift, abnormal speech or other neurological deficit; (b) administering tPA to said patient if said acute facial paresis, arm drift, or abnormal speech is observed and said quantity of said NR2 peptide is above the population norm for NR2 peptide in said biological fluid in apparently healthy human subjects; and (c) not administering tPA to said patient if said acute facial paresis, arm drift, or abnormal speech is not observed and said quantity of said NR2 peptide is below the population norm for NR2 peptide in said biological fluid in apparently healthy human subjects.
[0060] Moreover, one can periodically repeat the procedure to provide continuous monitoring of a patient's state as a follow up to treatment or to monitor the efficacy of a particular therapeutic regime. In this embodiment, it is preferable for the mammal to be concurrently undergoing treatment for the disorder. More preferably, the samples are collected at intervals from about 20 min to about 1 month. Even more preferably, the interval is from about 20 min to about 2 hours. Most preferably the samples are collected at an interval of about 30 minutes. Thus, in still another embodiment the invention provides a method for diagnosing the progression of cerebrovascular disorder, TIA or stroke further comprising measuring the presence or quantity of unbound and bound or total NR2 peptide and/or NMDA receptor fragments in a biological sample one or more additional times, at a frequency of less than about 6 hours. Once again, this testing is preferably performed in conjunction with NIHSS evaluations and neuroimaging. Put another way, in a still further embodiment, NR2 peptide is detected and quantified in a biological fluid from said patient a second time to obtain a second quantity of NR2 peptide; said second quantity of NR2 peptide is compared to said first quantity; tPA is administered a second time to said patient if the second quantity is greater than the first quantity; and tPA is not administered a second time to said patient if said second quantity is not greater than the first quantity.
Primary Care Physician Setting
[0061] In another application the method is used in a clinical setting to identify individuals who are at high risk in the near term of suffering a stroke, or to monitor the effectiveness of risk reducing therapies. A number of therapies can be employed to reduce the risk of stroke in an individual. The use of antiplatelet agents, particularly aspirin, is a standard treatment for patients at risk for stroke. People with atrial fibrillation (irregular beating of the heart) may be prescribed anticoagulants. When a treatment is prescribed, the methods provide a novel method for determine the efficacy of the therapy.
[0062] Therefore, in one embodiment the invention provides a method for evaluating an individual's risk for TIA or stroke comprising measuring levels of bound or total (and optionally unbound) NR2 peptide and/or NMDA receptor fragments thereof in a biological sample from the individual, and comparing the concentrations detected to a baseline level. In one embodiment the baseline levels are derived from population averages. In another embodiment the baseline levels are derived from the individual's own medical history in conjunction with NIHSS and DWI/MRI data.
[0063] In another embodiment the method is performed more than once to monitor the reduction or increase in risk for stroke or TIA, optionally in conjunction with the administration of risk reduction therapy (neuroprotective strategy). In one embodiment the method is performed at a frequency of from about once a week to about once in six months. In another embodiment the method is performed at a frequency of from about once in a month to about three months.
Pre-Surgery Risk Assessment
[0064] In still another embodiment the invention provides a method for aiding in the assessment of the risk of stroke in an apparently healthy human subject prior to surgery. When a patient is tested and has dangerous levels of bound or total NR2 peptides in his or her bloodstream, it is preferred to test the patient several more times before surgery and during surgery. In addition, because patients often do not suffer an adverse neurological event until shortly after the surgery, it is preferred to test these patients one or more additional times after surgery, within one or more of the following time periods: one hour, three hours, six hours, twelve hours, twenty four hours, three days, seven days, or thirty days.
[0065] The methods can be performed on adults or children scheduled for surgery, and are particularly useful when evaluating patients who are already predisposed to suffering a neurological event, such as patients with a history of diabetes, atherosclerosis, high blood pressure, or a previous suspected or confirmed TIA or stroke. The methods can also be used in conjunction with MMSA testing, before surgery, to predict the risk of an adverse neurological event. Preoperative decreased MMSA component scores for orientation, attention and recall have been associated with confusion and cerebrovascular events shortly after surgery.
[0066] The types of neurological events that can be predicted by the current invention are generally those induced by cerebral ischemia, and especially ischemic events that are caused by insufficient supplies of oxygen to the brain (as opposed to hemorrhagic events that occur when blood vessels are ruptured in the brain). These events can be focalized in a particular region of the brain, as occurs in stroke or TIA, or global, as occurs in delirium. The adverse neurological event may thus be characterized by confusion or may be diagnosed as a TIA or ischemic stroke. Oxygen supplies can be compromised due to the health condition of the patient (as in certain blood disorders such as anemia), but more commonly will be caused by the surgical event. The adverse neurological event is said to be “from” the surgery if the event occurs during surgery, or within thirty days after the surgery is completed, although the resulting adverse event could also be identified in a time frame of seven days, three days, two days or one day, if desired.
[0067] The prognostic methods of the present invention can predict the risk of adverse neurological events from any type of surgery, although traumatic surgeries that temporarily slow or halt the flow of oxygen to the brain will benefit most, For example, the method should be performed before any cardiovascular procedure that occludes or blocks normal blood circulation, that results in intraoperative micro- or macro-emboli, abnormal cerebral perfusion, reperfusion injury, or an inflammatory or neruhumoral response. The invention is especially useful in predicting the occurrence of adverse neurological events when a cardiopulmonary bypass is performed.
Diagnostic Platforms
[0068] The diagnostic methods for measuring bound or total NR2 peptide usually require the bound peptide to be stripped from any complexes in the bloodstream where the peptide is present, such as immunoglobulin and albumin complexes. This stripping is typically accomplished through the use of a protein detergent. Thus, in one embodiment, the invention provides a test kit for detecting and quantifying bound or total NR2 peptide in a biological sample comprising: (a) an antibody reagent comprising antibodies that are capable of specifically binding NR2 peptide in a test sample; (b) a protein detergent; and (c) an indicator reagent. In another embodiment the invention provides a method for detecting and quantifying bound or total NR2 peptide in a biological sample comprising: (a) contacting a biological sample with a protein detergent to yield a denatured biological sample; (b) contacting said denatured biological sample with an antibody reagent comprising antibodies that are capable of specifically binding NR2 peptide in a test sample, for a time sufficient to allow formation of bound complexes between said NR2 peptide and said antibody; and (c) detecting and quantitating said bound complexes.
[0069] The diagnostic methods of the present invention can be performed using any number of known diagnostic techniques, including direct or indirect ELISA, RIA, immunodot, immunoblot, latex aggutination, lateral flow, fluorescence polarization, and microarray. In one particular embodiment, the invention is practiced using an immobilized solid phase for capturing and measuring the NMDAR peptide marker. Therefore, in one embodiment the methods of the invention comprise: (a) contacting a biological sample from the patient with an immobilized solid phase comprising a NMDAR peptide or antibody, for a time sufficient to form a complex between said NMDAR peptide or antibody and NMDAR antibody or peptide in said biological sample; (c) contacting said complex with an indicator reagent attached to a signal-generating compound to generate a signal; and (d) measuring the signal generated. In a preferred embodiment, the indicator reagent comprises chicken anti-human or anti-human IgG attached to horseradish peroxidase.
[0070] In a preferred embodiment, the solid phase is a polymer matrix. More preferably, the polymer matrix is polyacrylate, polystyrene, or polypropylene. In one preferred embodiment the solid phase is a microplate. In another preferred embodiment, the solid phase is a nitrocellulose membrane or a charged nylon membrane.
[0071] In another embodiment, the method is performed using agglutination. Therefore, in still another embodiment the invention comprises: (a) contacting a biological sample from the patient with an agglutinating carrier comprising a NMDAR peptide or antibody, for a time sufficient to form an agglutination complex between said NMDAR peptide or antibody and NMDAR antibody or peptide in said biological sample; (c) generating a signal from the agglutination; (d) correlating said signal to said levels of one or more markers of NMDAR peptide or antibody. In a preferred embodiment, the “sufficient time” is less than 30, 20, 15 or even 10 minutes.
[0072] Latex agglutination assays have been described in Beltz, G. A. et al., in Molecular Probes: Techniques and Medical Applications, A. Albertini et al., eds., Raven Press, New York, 1989, incorporated herein by reference. In the latex agglutination assay, antibody raised against a particular biomarker is immobilized on latex particles. A drop of the latex particles is added to an appropriate dilution of the serum to be tested and mixed by gentle rocking of the card. With samples lacking sufficient levels of the biomarkers, the latex particles remain in suspension and retain a smooth, milky appearance. However, if biomarkers reactive with the antibody are present, the latex particles clump into visibly detectable aggregates.
[0073] An agglutination assay can also be used to detect biomarkers wherein the corresponding antibody is immobilized on a suitable particle other than latex beads, for example, on gelatin, red blood cells, nylon, liposomes, gold particles, etc. The presence of antibodies in the assay causes agglutination, similar to that of a precipitation reaction, which can then be detected by such techniques as nephelometry, turbidity, infrared spectrometry, visual inspection, colorimetry, and the like.
[0074] The term latex agglutination is employed generically herein to refer to any method based upon the formation of detectable agglutination, and is not limited to the use of latex as the immunosorbent substrate. While preferred substrates for the agglutination are latex based, such as polystyrene and polypropylene, particularly polystyrene, other well-known substrates include beads formed from glass, paper, dextran, and nylon. The immobilized antibodies may be covalently, ionically, or physically bound to the solid-phase immunoadsorbent, by techniques such as covalent bonding via an amide or ester linkage, ionic attraction, or by adsorption. Those skilled in the art will know many other suitable carriers for binding antibodies, or will be able to ascertain such, using routine experimentation.
[0075] Conventional methods can be used to prepare antibodies for use in the present invention. For example, by using a peptide of a NMDA protein, polyclonal antisera or monoclonal antibodies can be made using standard methods. A mammal, (e.g., a mouse, hamster, or rabbit) can be immunized with an immunogenic form of the peptide which elicits an antibody response in the mammal. Techniques for conferring immunogenicity on a peptide include conjugation to carriers or other techniques well known in the art. For example, the peptide can be administered in the presence of adjuvant. The progress of immunization can be monitored by detection of antibody titers in plasma or serum. Standard ELISA or other immunoassay procedures can be used with the immunogen as antigen to assess the levels of antibodies. Following immunization, antisera can be administered and, if desired, polyclonal antibodies isolated from the sera.
[0076] To produce monoclonal antibodies, antibody producing cells (lymphocytes) can be harvested from an immunized animal and fused with myeloma cells by standard somatic cell fusion procedures thus immortalizing these cells and yielding hybridoma cells. Such techniques are well known in the art, (e.g., the hybridoma technique originally developed by Kohler and Milstein (Nature 256, 495-497 (1975)) as well as other techniques such as the human B-cell hybridoma technique (Kozbor et al., Immunol. Today 4, 72 (1983)), the EBV-hybridoma technique to produce human monoclonal antibodies (Cole et al. Monoclonal Antibodies in Cancer Therapy (1985) Allen R. Bliss, Inc., pages 77-96), and screening of combinatorial antibody libraries (Huse et al., Science 246, 1275 (1989)). Hybridoma cells can be screened immunochemically for production of antibodies specifically reactive with the peptide and the monoclonal antibodies can be isolated. Therefore, the invention also contemplates hybridoma cells secreting monoclonal antibodies with specificity for NMDAR proteins or fragments as described herein.
[0077] In one embodiment the method is practiced using a kit that has been calibrated at the factory based upon antibodies purified from human blood. Therefore, in another embodiment the invention is practiced under the following conditions: (a) NMDAR antibody levels in said biological fluid are measured using a diagnostic kit; (b) said diagnostic kit comprises bound NMDAR peptides; and (c) said kit is manufactured against an antibody standard comprising a fraction of immunoglobulins G purified from human blood.
[0078] In addition, the method can be practiced using commercially available chemiluminescence techniques. For example, the method could employ a two-site sandwich immunoassay using direct chemiluminescent technology, using constant amounts of two monoclonal antibodies. The first antibody, in a fluid reagent, could be an acridinium ester labeled monoclonal mouse anti-human NMDA receptor peptide BNP (F(ab′) 2 fragment specific to a first portion of the peptide. The second antibody, in the solid phase, could be a biotinylated monoclonal mouse anti-human antibody specific to another portion of the peptide, which could be coupled to streptavidin magnetic particles. An immuno-complex would be formed by mixing a patient sample and the two antibodies. After any unbound antibody conjugates are washed away, the chemiluminescence of the immuno-complex signal could then be measured using a luminometer.
[0079] When the NMDA receptors are detected indirectly, by measuring the cDNA expression of the NMDA receptors, the measuring step in the present invention may be carried out by traditional PCR assays such as cDNA hybridization, Northern blots, or Southern blots. These methods can be carried out using oligonucleotides encoding the polypeptide antigens of the invention. Thus, in one embodiment the methods of this invention include measuring an increase of NMDAR cDNA expression by contacting the total DNA isolated from a biological sample with oligonucleotide primers attached to a solid phase, for a sufficient time period. In another preferred embodiment, NMDAR cDNA expression is measured by contacting an array of total DNA bound to a solid matrix with a ready-to-use reagent mixture containing oligonucleotide primers for a sufficient time period. Expressed NMDAR cDNA is revealed by the complexation of the cDNA with an indicator reagent that comprises a counterpart oligonucleotide to the cDNA attached to a signal-generating compound. The signal-generating compound is preferably selected from the group consisting of horseradish peroxidase, alkaline phosphatase, urinase and non-enzyme reagents. The signal-generating compound is most preferably a non-enzyme reagent.
[0080] The immunosorbent of the present invention for measuring levels of autoantibody can be produced as follows. A fragment of the receptor protein is fixed, preferably by covalent bond or an ionic bond, on a suitable carrier such as polystyrene or nitrocellulose. If the standard polystyrene plate for immunological examinations is employed, it is first subjected to the nitration procedure, whereby free nitrogroups are formed on the plate surface, which are reduced to amino groups and activated with glutaric dialdehyde serving as a linker. Next the thus-activated plate is incubated with about 2 to 50 nM of the target peptide for the purpose of chemically fixing the respective immunogenic fragment of the receptor protein for a time and at a temperature sufficient to assure fixation (i.e. for about 16 hours at 4° C.).
[0081] It is also practicable to produce the immunosorbent by fixing the respective fragment of the receptor protein on nitrocellulose strips by virtue of ionic interaction. The respective fragment of the receptor protein isolated from the mammals' brain is applied to nitrocellulose and incubated for 15 min at 37° C. Then nitrocellulose is washed with a 0.5% solution of Tween-20, and the resultant immunosobent is dried at room temperature and stored in dry place for one year period.
Examples
[0082] The following examples are put forth so as to provide those of ordinary skill in the art with a complete disclosure and description of how the compounds claimed herein are made and evaluated, and are intended to be purely exemplary of the invention and are not intended to limit the scope of what the inventors regard as their invention. Efforts have been made to ensure accuracy with respect to numbers (e.g., amounts, temperature, etc.) but some errors and deviations should be accounted for. Unless indicated otherwise, parts are parts by weight, temperature is in ° C. or is at room temperature, and pressure is at or near atmospheric.
Example 1
Patient Groups Studied
[0083] Forty one adult patients with symptoms suggestive of a possible transient ischemic attack and at high risk in the near term for a completed stroke (Table 1) were evaluated. Exclusion criteria included those patients whose symptoms resolved after treatment with glucose and were likely suffering from hypoglycemia.
[0084] During routine evaluation of the patient, the evaluating physician verified the presence or absence of five factors including: age >60, diabetes mellitus, TIA symptoms >10 minutes, weakness, speech impairment. After informed consent, blood samples were collected on the day of admission from all subjects. Patients were then followed-up approximately ninety days after presentation via telephone, personal interview, or review of medical records to assess for recurrent TIA or stroke. Stroke was defined as having occurred if a patient developed a permanent neurological deficit or new radiographic (CT or MRI) evidence of central nervous system infarct correlating with the patient's symptom onset during the ninety days following initial evaluation. The multi-sequence MR imaging protocol, which included DW1, T2WI and MRA, was performed as a single session within 24 hours after symptom onset. The following CT imaging data were recorded: location of hemorrhage, hemorrhage volume, and presence of intraventricular blood or mass effect. The amounts of unbound NR2 peptide were determined in plasma of the above described patients and an age-matched group of healthy volunteers (n=10).
[0085] One patient was excluded after showing basal ganglia growth and being diagnosed with a brain tumor (Table 1). 42% of patients underwent MRI examination within 3 hours of symptom onset, and 79% of patients underwent CT scanning within 3 hours of symptom onset.
[0000]
TABLE 1
Demographic Characteristics of patients
Characteristics
Baseline
Mean age, y
65.0
Men, n
20
Left side of body event, n
13
Mean initial blood glucose, mg/dL
151
Example 2
Unbound NR2 Peptide as a Marker of New Brain Lesions
[0086] Concentrations of unbound NR2 peptide in blood were obtained by direct ELISA as presented in Table 2. The distribution of unbound NR2 peptide depicted in FIG. 1 showed that patients with values of unbound NR2 peptide below 1.0 ng/ml (n=16) had no area of damage defined by CT/MRI (Table 1). The plasma of healthy persons had concentrations of unbound NR2 peptide ranging from 0.3 to 0.5 ng/ml.
[0000]
TABLE 2
Unbound NR2 peptide in plasma of patients studied
Unbound NR2
Subjects
peptide range
Neuroimaging
N
(min, max), ng/ml
Diagnosis
modality: CT/MRI/DWI
16
0.3-1.0
CVA, radial &
Negative or hemorrhage
Bell's palsies,
on CT
ICH
14
1.0-44.0
based on NIHSS:
New lesions in cortex,
TIA, stroke
subcortical areas,
cerebellum, thalamus,
lacunar
[0087] Concentrations of unbound NR2 peptide above 1.0 ng/ml were detected in plasma of patients (n=14) with new ischemic lesions located in the cortex, basal ganglia, cerebellum and thalamus defined by DWI/MRI. (Table 2). In three patients with ischemic stroke (IS) abnormally elevated concentrations of unbound NR2 peptide allowed the diagnosis of lacunar infarcts that were then defined by DWI.
Example 3
Total NR2 Peptide as a Marker of Old Brain Lesions
[0088] Serum samples from 40 patients with suggestive TIA were analyzed for total NR2 peptide amounts (Table 3).
[0000]
TABLE 3
Amounts of total NR2 peptide in serum of patients studied
Total NR2
Subjects
peptide range
Neuroimaging
N
(min, max), ng/ml
Diagnosis
modality CT/MRI/DWI
17
0.9-2.0
CVA, radial &
Negative or hemorrhage
Bell's palsies,
on CT
ICH
14
2.4-24.0
based on NIHSS:
Old parietal infarct,
TIA, stroke
mid white matter,
lateral ventricle,
MCA area
[0089] The statistical analysis of data showed that most patients had total NR2 peptide concentrations below 2.0 ng/ml ( FIG. 2 ). Healthy persons had total NR2 peptide concentrations of 1.0-1.5 ng/ml. Neuroimaging of patients did not show abnormalities except for those with ICH. Concentrations of total NR2 peptide were >2.4 ng/ml in patients with previous history of cerebral ischemia and old infarction areas defined by MRI (Table 3). Nine patients out of 40 were clinically diagnosed as having recurrent TIA or stroke.
Example 4
Unbound and Total NR2 Peptide in Patients with TIA/Stroke (Primary and Recurrent Symptoms)
[0090] The simultaneous detection of unbound and total NR2 peptide allowed differentiation of patients with recurrent TIA/stroke from patients having new areas of infarction. Table 3 presents gives clinical diagnoses in patients based on CT/MRI/DWI, compared to their total and unbound NR2 peptide levels. Patients (n=14) with infarction areas on MRI/DWI had “old” areas of lesions and a ratio of unbound:total peptides of less than 1:2 (Table 3, cases 3, 13, 16, 21).
[0000]
TABLE 3
Unbound/total NR2 peptide in patients studied
NR2 peptide, ng/ml
Case
Unbound
Total
Ratio
CT/MRI/DWI
3
1.1
2.85
1:2.6
Old right MCA stroke on CT and
MRI
13
1.22
2.4
1:2.0
Small infarctions in
pontomidcephalic region
16
1.30
8.8
1:6.8
MRI showed lacunar infarcts
21
1.11
2.35
1:2.0
Old parietal infarct and some
lacunar infarcts on DWI
32
8.3
0.8
10:1
Acute left cerebellar infarction
(new)
35
24.5
1.2
20:1
Acute left upper pons lesions (new)
[0091] The patients who had drastically increased unbound NR2 peptide in plasma all had total peptide concentrations below 2.0 mg/ml, and all suffered from acute stroke with new areas of lesions defined by MRI/DWI (Table 3, cases 32, 35). The ratio of unbound:total NR2 peptides in the two patients were both greater than 2:1.
Example 5
The Correlation of Unbound/Total NR2 Peptide with NIHSS
[0092] On admission NIHSS scores were assessed in 40 patients who were then subdivided into two groups—those with NIHSS scores less than or equal to three, and those with NIHSS scores greater than three (Table 4). An MRA was completed in all patients; 24 of the 40 patients had evidence of flow abnormalities. There was no statistical difference in the proportion of patients who had CT or MRI within 3 hours of symptom onset or in the hemisphere of stroke between the NIHSS≦3 and the NIHSS>3 groups.
[0000]
TABLE 4
Demographic Characteristics of NIHSS
≦ 3 with NIHSS > 3 Groups
NIHSS ≦ 3,
NIHSS > 3,
(n = 26)
(n = 14)
Mean age, y
64.3
65.5
Median NIHSS
3
16
Men, n
11
9
Left side of body event, n
3
10
Mismatch on MR, n
2
6 (n = 11)
[0093] Only 5 patients out of 24 patients had NIHSS scores less than or equal to three. None of these 5 patients had symptoms suggestive of a lacunar syndrome. Of the 5 patients, 4 had evidence of DWI changes. Unbound NR2 peptide above the 1.0 ng/ml cutoff was detected in the plasma of 3 patients (Table 5), while total NR2 peptide remained under the 2.0 ng/ml cut off for all persons who were diagnosed with TIA.
[0000]
TABLE 5
Breakdown of 5 Patients With NIHSS < 3 + primary TIA
NR2 peptide, ng/ml
NIHSS
Case
Unbound
Total
Baseline
Hemisphere
19
0.79
0.9
3
Right
38
1.50
2.0
2
Left
7
1.85
1.7
2
Left
9
2.85
1.1
3
Right
36
0.79
1.8
3
Left
[0094] The remaining 19 of 24 patients had NIHSS greater than three, and evidence of a DWI lesion at baseline. Within this group 5 patients were diagnosed with chronic TIA, and the remaining 14 patients were diagnosed as having acute IS. There was a significant correlation (r s =0.92) between the NIHSS scores and values of unbound/total NR2 peptide. Patients later diagnosed as having acute IS (n=9) and NIHSS scores of 11-20 had unbound NR2 peptide levels approximately 3-44 times higher than levels observed in control subjects. The level of total NR2 peptide and median NIHSS scores had significant correlation (r s =0.89) for patients with chronic TIA and recurrent IS (n=14).
Example 6
Unbound/Total NR2 Peptide in Patients with Stroke-like Disorders
[0095] Within the group of persons evaluated who demonstrated TIA-like symptoms (n=16), two patients were diagnosed with Bell's and radial nerve palsies and three patients were diagnosed with intracerebral hemorrhage (ICH). In those patients unbound NR2 peptide was below the 1.0 ng/ml cutoff and total NR2 peptide was below the 2.0 ng/ml cutoff (Table 6). The preliminary diagnosis for case 34 was cerebrovascular disorder, but this diagnosis was changed to intracerebral hemorrhage after NR2 peptide testing and additional CT tests.
[0000]
TABLE 6
Unbound/total NR2 peptide in patients with stroke-like disorders
NR2 peptide, ng/ml
Case
Unbound
Total
Diagnosis
CT/MRI/DWI
15
0.66
1.9
Bell's palsy
Negative
17
0.45
2.0
ICH
ICH on CT
24
0.67
1.3
ICH
ICH on CT
33
0.30
1.0
Radial nerve palsy
Negative
34
0.28
1.2
ICH
ICH on CT
27
1.21
0.8
Bell's palsy changed
Left thalamus
to TIA
lacunar infarcts
8
0.68
24.0
Migraine changed to IS
Lacunar infarcts
[0096] Case 27 showed unbound/total NR2 peptide under the corresponding cutoffs, but the preliminary diagnosis “Bell's palsy” was changed to “TIA” after DWI revealed lacunar infarct areas in thalamus. Case 8 was initially characterized as severe migraine but changed to ischemic stroke based on the results of total and unbound NR2 peptide testing. The DWI imaging detected lacunar lesions in the brain confirming the diagnosis of acute IS.
Example 7
Plasminogen Activator Treatment
[0097] A total of 13 patients with primary/chronic TIA and new/recurrent stroke were treated with plasminogen activator (tPA) within 24 h of admission (Table 7). Two patients had NIHSS scores less than three, were diagnosed as having primary TIA, and recovered within 24 h of admission without receiving thrombolytic therapy. Three patients received tpA in a dose of 66 mg after their NIHSS scores worsened by 1-2 points in the first 24 hours (cases 19, 36, 38).
[0098] Unbound NR2 peptide levels decreased substantially after tPA treatment (Table 8). The following assessment demonstrated their independency on the modified Rankin Scale at 3 months (Table 7).
[0000]
TABLE 7
Patients treated with tPA
NIHSS
3-month Rankin
N
Case
Baseline
24-h
Diagnosis
Scale Score
1
19
3
3
Primary
Independent
2
38
2
4
TIA
Independent
3
36
5
7
Independent
4
11
7
5
Recurrent
Symptoms recurrence
5
12
5
3
TIA
Independent
6
13
9
4
Independent
7
32
15
12
New cerebral
Independent
8
35
18
14
ischemia
Independent
9
3
11
7
Recurrent IS
Independent
10
8
20
16
Independent
11
10
17
14
Delirium at 2 mo.
12
16
19
16
Independent
13
25
16
12
Independent
[0099] Patients with chronic TIA who had areas of lesion defined by DWI, and who did not show improvement in symptoms within 3 hours of admission, received intravenous tPA (66 mg) and this administration caused an improvement in NIHSS scores (Table 7). The clinical improvement was accompanied by a reduction of total and unbound NR2 peptide concentrations (Table 8). The most significant improvements in NIHSS scores were associated with greater reductions in total NR2 peptide concentrations compared to unbound NR2 peptide concentrations. Symptoms reoccurred for case 11 within three months.
[0000]
TABLE 8
Alteration of unbound/total NR2 peptide after tPA administration
Unbound NR2 peptide
ng/ml
Total NR2 peptide, ng/ml
N
Case
Baseline
24-h
Baseline
24-h
1
19
0.79
0.53
0.9
1.1
2
38
0.79
0.50
1.8
1.9
3
36
2.85
1.75
1.1
1.4
4
11
1.22
1.1
2.4
2.0
5
12
0.58
0.50
2.5
1.6
6
13
1.61
1.0
5.5
3.4
7
32
8.3
4.4
0.8
1.0
8
35
24.5
11.2
1.2
1.4
9
3
1.0
0.5
2.85
1.5
10
8
0.68
0.44
24.0
5.5
11
10
0.68
0.50
4.5
4.0
12
16
1.30
0.6
8.8
4.3
13
25
44.0
8.5
4.1
2.8
[0100] The timely tPA administration (within 3 hours of symptoms) among patients with new stroke (cases 32, 35) significantly reduced unbound NR2 peptide (38-47%) and patients were independent on the modified Rankin Scale at 3 months (Table 7). In spite of an initial improvement in NIHSS scores, and a slight decrease of unbound/total NR2 peptide concentrations for case 10 after tPA (69 mg) was administered within 6 hours of admission, the patient subsequently deteriorated over the next two months (Table 7, 8). Thrombolytic therapy reduced concentrations of unbound NR2 peptide up to 90% in case 25.
Example 8
Total and Unbound NR2 Peptide Detection Assays and Performance Characteristics
[0101] Coating of the ELISA plates. Nunc MaxiSorp plate (Fisher Sci) was coated by 0.2 μg of chicken anti-NR2 IgY in 100 μL of 15 mM sodium carbonate, 35 mM sodium bicarbonate, pH 9.6. Plates were incubated overnight and then treated by 200 μL of 1 M ethanolamine, pH 8-9 for 1 hour. After rinsing in PBS buffer the plates were subsequently stored at +4° C.
[0102] Blood sample preparation. Blood (1 ml) is collected by venipuncture in sterile disposable tubes from individuals. Each one-ml blood sample should be split evenly between EDTA tubes (plasma) and clot-activator tubes (serum). For plasma, the tubes are centrifuged at 4000 g for 5 min at 4° C. For serum, the blood is allowed to clot in the tube for 20 minutes and then centrifuged at 1000 rpm for 10 minutes. The collected plasma and serum should be stored at −70° C.
[0103] Samples Pre-dilution: pipette exactly 20 μL of each serum sample into 2-3 mL volume tubes and add 980 μL of 50 mM phosphate buffer, containing 0.05% Tween 20 (PBS-T), pH 7.4 (for unbound peptide assay) or 0.1-0.5% sodium dodecylsulphate solution (or KCl) prepared on PBS-T (for total peptide assay), mix thoroughly for 10-30 min.
[0104] Direct ELISA for peptide detection. For each assay, the plate should be washed for 5 min with PBS-T. Calibrator, control, or sample (100 μL) should be then added in duplicate and incubated for 60 min at room temperature (RT). After the plate is washed three times for 15 min, 100 μL of human IgG, (6 μg/well) should be added and incubated for another 60 min at RT. After washing with buffer, Protein A-HRP is added (100 μl; 1:1,000 dilution) for 1 hour.
[0105] The reaction is revealed by tetramethylbenzedine (TMB) substrate solution after additional washing. Color reaction is developed for 5 min, stopped with acid solution (50 μl) and monitored at dual wave 450 nm/630 nm on a microplate reader. Sample buffer is also included as the blank in each assay to calculate the zero unit value. The concentration of NR2 peptide in serum is determined using the calibration curve of absorbance units of NR2 peptide versus concentration in microplate wells.
Example 9
Performance Characteristics for Unbound/Total NR2 Peptide Assays
Unbound NR2 Peptide
[0106] Operating characteristics of unbound NR2 peptide are depicted in 2×2 format in Table 9. The sensitivity and specificity of 90% and 95% at 1.0 ng/ml cutoff were calculated. Predictive values and likelihood ratios at specific cutoff points were chosen to approximate the sensitivity of 90%. At the 1.0 ng/ml cutoff value for TIA/stroke diagnosis the positive predictive value of 95% was achieved resulting in a 18-fold increase (95% CI, 10.8-25.4) in post TIA neurological complications for patients with high levels of NR2 peptide. The negative predictive value of 90% and negative likelihood ratio- of 0.05 allow misdiagnosis of TIA/stroke only in 5% of cases with stroke-like symptoms. The unbound NR2 peptide values combined with DWI/MRI data should allow 100% identification of cerebral ischemia.
[0000]
TABLE 9
Unbound NR2 Peptide performance
True Positive
19
1
False Negative
False Positive
2
19
True Negative
21
20
Total NR2 Peptide
[0107] Operating characteristics of total NR2 peptide are presented in 2×2 format in Table 10. The lower sensitivity of 82% and about the same specificity of 96% at the 2.0 ng/ml cutoff were calculated for a total NR2 assay compared with an unbound peptide test. At the best 2.0 ng/ml cutoff value for TIA/stroke diagnosis, the positive predictive value of 93% was achieved resulting in a 20.5-fold increase in neurological complications for patients with high levels of total NR2 peptide. The negative predictive value of 88% and negative likelihood ratio of 0.18 allow misdiagnosis of TIA/stroke in 18% of cases with stroke-like symptoms. The simultaneous detection of unbound and total NR2 peptide combined with DWI/MRI data should allow 100% identification of cerebral ischemia and subdivision of cases between new and recurrent ischemic events.
[0000]
TABLE 10
Total NR2 Peptide performance
True Positive
14
1
False Negative
False Positive
3
23
True Negative
17
24
[0108] Throughout this application, various publications are referenced. The disclosures of these publications in their entireties are hereby incorporated by reference into this application in order to more fully describe the state of the art to which this invention pertains. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims. | Methods and kits for diagnosing and treating cerebrovascular events, and for defining the time and anatomical location of an event, are provided based on the detection and quantification of bound or total and unbound NR2 peptides in biological fluids. The methods are optionally performed in conjunction with neurological scoring and neuroimaging, and are directed to risk assessment, prognosis, diagnosis and treatment of TIA and stroke on an emergency basis in the emergency room. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention pertains to thermostatically controlled fittings for internal combustion engine coolant systems which includes a closable bypass passage which permits coolant flow therethrough during filling of the engine coolant system to eliminate trapped air pockets.
2. Description of the Related Art
Internal combustion engines utilize thermostatically controlled valves to regulate the coolant temperature for various purposes. Such thermostatic valves are closed when the engine is cold to prevent coolant circulation and accelerate the heating of the engine block to improve engine operating characteristics, and accelerate the heating of the vehicle occupant climate control system. Upon the engine coolant reaching a predetermined elevated temperature, the thermostatic valve begins to open permitting the coolant to circulate through a cooling radiator to achieve the desired coolant temperature during normal engine operation.
Such thermostatic valves may be incorporated into various parts of the engine coolant system. Usually, thermostatic valves are incorporated into hose lines or hose fittings for ease of assembly and replacement.
When an internal combustion engine is initially assembled, it is, of course, cold and the thermostatic valves in the coolant system will be closed. As the coolant is introduced into the coolant system, the closed thermostatic valve will cause air to be trapped within the coolant system preventing the coolant system from being fully charged with coolant, and it is often necessary to use expensive "bleeding" procedures to permit entrapped air to escape from the coolant system during the initial engine coolant charging. Due to the complexity of modern internal combustion engines, the confinement and clearance problems existing in the engine compartment, especially in front wheel drive vehicles, the loosening of components within the coolant system to permit the bleeding of entrapped air is difficult and time consuming, and once the bleeding has been completed, it is possible for the mechanic to overlook the need to fully restore the coolant system to its liquid tight condition resulting in liquid loss during engine operation.
OBJECTS OF THE INVENTION
It is an object of the invention to provide a fitting for internal combustion engine coolant systems which permits a cold engine to be fully charged with coolant regardless of the fact that the thermostatic valve within the fitting may be closed, and wherein the coolant system maintains its sealed integrity and coolant loss to the atmosphere is prevented.
Another object of the invention is to provide a fitting for the coolant system of internal combustion engines containing thermostatically controlled normally closed valves wherein the fitting consists of two parts which may be readily manipulated between coolant bleeding and normal operating positions and the fluid-tight integrity of the coolant system is maintained at all times.
Yet another object of the invention is to provide a fitting for an internal combustion engine coolant system having a normally closed thermostatic valve wherein the fitting parts may be economically manufactured, readily assembled, and the parts relatively movable between coolant bleeding and operative positions by an unskilled operator, and wherein the condition of the fitting may be readily observed.
SUMMARY OF THE INVENTION
The invention takes the form of a fitting to be located within an internal combustion engine coolant system. In the disclosed embodiment, the fitting is incorporated into the coolant hose system, but it is to be appreciated that the concepts of the invention may be incorporated into a coolant fitting partially formed by the engine block or associated component. In the practice of the invention, it is necessary that the coolant fitting consist of at least two parts, and one of the parts being relatively movable to the other requiring that the movable part be associated with a flexible hose incorporated into the cooling system.
The two parts constituting the fitting each include a coolant flow passage therethrough, and a conventional thermostatic normally controlled valve will be incorporated into one of the parts capable of associating with a valve seat whereby the valve controls fluid flow through the fitting assembled parts. In its normal "cold" condition, the valve will be closed preventing coolant flow between the fitting parts.
The fitting parts are interconnected by connection structure preferably of the bayonet type including tongues fitting within slots. In actuality, a plurality of slots and tongues are concentrically positioned with respect to an axis of relative rotation between the parts whereby relative part rotation causes a tongue to enter and cooperate with an associated slot to maintain the parts in assembled relationship.
The slots and tongues are configured such that their interrelationship is in two stages. The slots each include a pair of restraining surfaces for cooperation with the tongues which are axially spaced relative to each other wherein engagement between the tongues and the first restraining surface produces a first axial relationship between the parts, while further rotation of the parts causes the tongues to engage the second restraining surfaces within the slots further axially displacing the parts toward each other to a final fully connected condition.
An annular resilient flexible seal is interposed between the fitting parts at the connection structure adapted to be compressed upon the parts being fully connected, and the seal is received between opposed parts' surfaces to maintain a sealed relationship between the interior of the fitting parts and the atmosphere at both stages of interconnection between the parts thereby rendering the fitting fluid tight to the atmosphere regardless of the condition of the parts' interconnection between the two stages.
During the initial stage of parts' interconnection, the elastomeric seal does not seal the parts' flow passages relative to each other, as the plate in which the valve head is mounted not engaging its seal and the separation of the parts within the parts' flow passages permits a bypass passage to be defined around the valve permitting one part to communicate with the flow passage of the other part wherein air and coolant may flow from one fitting part to the other around the thermostatic valve. This condition of the fitting parts prevents air from being trapped on one side or the other of the valve providing a "bleed" condition to prevent air from being trapped within the coolant system and permitting the engine cooling system to be fully filled or charged with coolant.
After the engine coolant system has been fully filled, the two parts of the valve fitting may be relatively rotated causing the tongues to engage the second set of restraining slot surfaces drawing the parts closer together causing the plate in which the valve head is mounted to engage the elastomeric seal between the parts to close off the valve bypass passage and permitting coolant flow through the fitting only in accord with the position of the thermostatic valve.
While the relative angular rotation between the fitting parts between the two stages of interconnection is not great, the angular relationship between the fitting parts may be readily observed by the operator, and the condition of the fitting visually noted. If desired, index marks may be mounted on the fitting parts of a raised or recessed type to indicate the relative condition between the fitting parts, and if desired, indicia may be employed indicating "closed" and "bypass" positions. Rotation of the fitting parts relative to each other may be readily manually accomplished by an operator, even in cramped quarters, and requires minimal technical skills.
As a coolant fitting in accord with the invention prevents the escape of coolant to the atmosphere during the filling of the engine coolant system, environmental concerns are met, loss of expensive coolant is prevented and a highly desirable coolant filling process is achieved for internal combustion engines.
BRIEF DESCRIPTION OF THE DRAWINGS
The aforementioned objects and advantages of the invention will be appreciated from the following description and accompanying drawings wherein:
FIG. 1 is a diametrical sectional view of an internal engine coolant fitting utilizing the concepts of the invention, the fitting parts being shown in the fully closed condition,
FIG. 2 is a plan sectional view taken along Section 2--2 of FIG. 1,
FIG. 3 is an enlarged sectional view of the interconnection between the fitting parts as taken along Section 3--3 of FIG. 2, illustrating the parts in the initial coolant charging position when the bypass flow passage is open,
FIG. 4 is an enlarged detail sectional view similar to FIG. 3 illustrating the relationship of the fitting parts when fully assembled,
FIG. 5 is an elevational detail view of the fitting parts bayonet slots and tongue illustrating the relationship of the components during the partially connected engine coolant charging condition,
FIG. 6 is an enlarged detail elevational view similar to FIG. 5 illustrating the fitting parts in the fully connected position,
FIG. 7 is a perspective view of the components shown in FIG. 5 during partial parts interconnection, and
FIG. 8 is a perspective view of the components shown in FIG. 6 during full connection.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to FIG. 1, a fitting for an internal engine cooling system is generally indicated at 10, and the fitting basically consists of a first part 12 connected to a second part 14 through connection structure generally indicated at 16. The fitting 10 may be formed of metal or a synthetic plastic material, and is incorporated into the hose system of the coolant circuit of an internal combustion engine, not shown.
The part 12 is hollow and includes an internal flow passage 18 communicating with the tubular nipple 20 upon which a hose, not shown, constituting a part of the coolant system circuit is mounted and clamped.
A thermostatic valve 22 is located within the flow passage 18 and the valve includes a valve stem 24 terminating in a valve head located within a plate 26. The valve 22 senses the temperature of the engine coolant, and the entire fitting 10 may be connected to the engine block through a valve cap 28 whereby the valve 22 is directly exposed to the temperature of the engine block. In its normal condition, the valve 22 will be expanded which extends the valve head within plate 26 downwardly as shown in FIG. 1, and as the temperature of the coolant increases, the valve head within plate 26 will rise. As is well known, thermostatic valves 22 are pre-set to open and close at predetermined temperatures depending on the engine coolant system design.
The part 12 includes an annular lower flange 30 having a plurality of radially extending tongues 32 defined thereon, three tongues being shown in the illustrated embodiment. Each of the tongues 32 includes a forward portion 34 transversely disposed to the axis of the connection structure 16, and concentric to such axis. The tongues also include a transitional or inclined cam portion 36 which extends from portion 34 and blends with rear portion 38. As will be appreciated from the drawings, the portions 34 and 38 are axially offset with respect to each other, and the forward portion 34 constitutes the primary connection to the part 14.
The fitting part 14 includes a flow passage 44 communicating with the tubular nipple 46 adapted to receive a hose and clamp, not shown, constituting a part of the engine coolant system. The part 14 includes an annular valve seat extension 48 adjacent the connection structure 16 and the upper end of the extension 48 constitutes a valve plate stop at 50. The lower flange 30 of part 12 is radially spaced outwardly with respect to the valve seat extension 48 defining an annular chamber 54 between the extension 48 and flange 30. The annular chamber 54 includes a ridge 56 formed in the part 14 and an annular resilient flexible O-ring type seal 58 is received within the chamber 54. The diameter of the cross section of the seal 58 is slightly greater than the radial dimension of the chamber 54 whereby the seal provides a fluid tight sealing between the extension 48 and flange 30 preventing the loss of coolant to the atmosphere at either connection stage of the parts 12 and 14 as later described.
A plurality of slots 59 are formed upon the part 14 within the annular boss 60 constituting a portion of the connection structure 16 and as three tongues 32 are defined on the part 12, three similar slots 59 are formed upon the part 14 of such a dimension and configuration as to receive the tongues 32. Each slot 59 includes an initial connection retainer surface 62, a transition cam surface portion 64 and a final connection retainer surface 66.
A detent recess or groove 68 is defined in the surface 62, while a detent recess 70 is defined in the retainer surface 66 and upon the upper surface of the tongue forward portion 34, as shown in FIGS. 5 and 6, a detent projection 40 extends capable of being selectively received within recesses 68 and 70.
A plurality of ribs 72 are formed in the flange 30 at the connection structure 16 and these vents are circumferentially spaced about the interior of the flange to define a plurality of passages 74 therebetween. The passages 74 as defined by the radial dimension of the ribs 72 is greater than the diameter of the plate 26 in which valve head is located whereby fluid may flow around the periphery of the plate 26 between the ribs 72 when the parts 12 and 14 are partially or preliminarily interconnected,
In the use of the fitting 10, the appropriate coolant system hoses, not shown, will be mounted upon the fitting nipples 20 and 46, and the parts 12 and 14 will be preliminarily assembled wherein the tongues 32 will be received within the slots 59 and the tongues' forward portions 34 will be disposed "under" the slots' retainer surfaces 62. The detent 40 will be received within the detent recesses 68 as shown in FIGS. 5 and 7.
In this relationship of the components, the extension 48 and flange 30 will be in radial opposed relationship as shown in FIG. 3, and the seal 58 will prevent coolant within the fitting 10 from escaping to the atmosphere. However, due to the axial separation of the surfaces 62 and 66 with respect to the axis of rotation of the connection structure 16 the plate 26 will not be engaging the seal 58, and coolant may flow from the flow passage 44 of part 14 to the flow passage 18 of the part 12 around the periphery of the plate 26 between the ribs 72 as shown by the arrows 76, FIG. 3. This bypassing of the plate 26 through the passages 74 permits any air that may be trapped within the part 14 to escape from below the plate 26 into the part 12 and through the connected hose and, of course, such air will flow to the upper portion of the coolant system and escape to the atmosphere. Accordingly, the components of the fitting 12 will be maintained in the partially connected condition shown in FIGS. 3, 5 and 7 during filling of the engine coolant system thereby preventing thermostatic valves within the system from entrapping air.
After the engine coolant system has been completely charged, the mechanic will then rotate the parts 12 and 14 relative to each other causing the tongues 32 to engage the slot cam surface 64 and position the tongues' forward portions 34 against the slots' retaining surfaces 66 as shown in FIGS. 6 and 8. In this condition, the detent 40 will be received within the detent recess 70. This relative rotation of the parts 12 and 14 about the axis of the connection structure 16 will force the parts 12 and 14 toward each other and the plate 26 in which the valve head is mounted will engage the seal 58 as shown in FIG. 4. When the valve plate 26 engages the seal 58 the passages 74 become sealed, and fluid flow between the parts 12 and 14 is prevented by the plate 26 and seal 58, and when the coolant heats to the desired temperature and the valve head opens and lifts within the plate 26 during the normal temperature controlling operation of the valve 22 and the coolant will flow through passages 74.
The engagement of the detent 40 with the recess 70 prevents inadvertent disassembly of the parts 12 and 14 due to vibration, and the components will remain in this locked condition during the normal engine operation. If the coolant system is drained, and it is desired to permit bleeding through the fitting 10, the parts 12 and 14 may be rotated to the position shown in FIGS. 5 and 7, and the coolant system again charged as described above.
The angular relationship between the parts 12 and 14 may be readily observed by the mechanic, and accordingly, the condition of the fitting 10 is readily observable. As the seal 58 prevents coolant leakage from the fitting during both the preliminary and final connection of the fitting parts, loss of coolant is prevented, and a coolant fitting constructed in accord with the invention overcomes many of the problems previously encountered with respect to engine coolant charging.
To aid in determining the angular relationship between the parts 12 and 14, indicia or index marks may be formed upon the parts so as to be relatively comparable. Such index marks may be raised or recessed, molded or cast into the parts, and may include terminology such as "closed" or "bypass". Also, it is to be understood that the nipples 20 and 46 may take various forms, and could include automatic self-connecting fittings whereby the hose may be readily plugged onto the parts 12 and 14 without requiring hose clamps.
It is appreciated that various modifications to the inventive concepts may be apparent to those skilled in the art without departing from the spirit and scope of the invention. For instance, rather than the valve bypass passage being defined by the partial open condition of the thermostatic valve during the initial interconnection of the parts, as described, a separate bypass passage could be defined in one or both of the parts which is open during the first stage of parts' interconnection and closed during the final connection of the parts, and such a variation is within the scope of the invention. | An internal combustion engine fitting containing a thermostatically controlled valve regulating the flow therethrough is formed by two parts interconnectable by relative rotation through a bayonet type connection. The bayonet connection utilizes two stages wherein the first stage maintains the parts connected but a bypass passage defined between the parts permits the flow of coolant through the fitting around the valve to initially permit the engine coolant system to be filled. After the coolant system is filled, the fitting parts are rotated to a final closed position sealing the bypass passage permitting the thermostatic valve to control flow through the fitting during normal engine operation. The fitting parts remain sealed to the atmosphere during both stages of interconnection. | 8 |
FIELD OF THE INVENTION
This invention relates to the spring retention of assemblies of articles, for example the retention of curved ceramic permanent magnets to the inside wall of a steel motor housing ring.
BACKGROUND OF THE INVENTION
It is often desirable or necessary to retain equipment components without threading, piercing or otherwise re-working one of the components. Securing ceramic magnets in a steel housing ring for permanent magnet motors is one example. Spring retainer clips and adhesives are common means for accomplishing this objective.
Adhesive techniques and materials offer a wide variety of approaches for securing articles to one another. However, there are inherent disadvantages including the time required and the special equipment needed for curing the adhesive; the handling, mixing, applying, and cleaning up of the adhesive; and precautions against noxious or toxic effects. Further, the costs of special quick-drying adhesives and related special equipment, and the troubles of maintaining the necessary tight control of surface tolerances are often significant. To avoid these, sometimes assemblies are secured with the use of both an adhesive and retainer clips. The retainer clips may be removed after the adhesive has set, or they may be left in permanently, depending upon individual economic and structural considerations.
The use of spring retainers in lieu of adhesives is desirable, where practical. In some cases, the spring retainers--typically bow or wave-shaped flat metal compression springs--are pressed or snapped into their final loaded position. In other applications the springs and magnets are assembled loosely in a larger diameter fixture, after which the assembly is compressed radially, and then axially inserted into the cylindrical housing.
There are a number of problems which limit the use and effectiveness of the existing spring retainer approaches. Variations in the arc lengths of the articles to be retained, and in dimensions of other mating components, pose difficulties with respect to critical relationships between the retainer spring's relatively short length, and the requirements for both sizeable loads and large tolerance take-up capabilities. Closer control of tolerances entails higher costs. Also, the pre-compression, as well as the snap-in assembly operations often tend to break or chip ceramic magnets or other brittle articles. In some instances, spring retention systems have been avoided and even abandoned because of concern for unacceptable breakage, or for displacement from impacts during assembly, handling, shipping or use.
The need remains for a basically improved mechanical retention system which is adaptable to:
a. large tolerance variations beyond the working length of ordinary springs;
b. providing sizeable, and consistent holding forces without damaging magnets or other parts being retained; and
c. easy and rapid manual or automatic assembly techniques (without contending with spring loads during assembly of components). The term "working" is sometimes used to describe the spring of this invention. It is in fact a spring which continues to exert a bias force adaptable both in compression and extension. The application of this force as retention means is merely one application, in which it resists cyclical vibratory forces and thermal expansion and compression as encountered in electrical motors, while still pressing against an article such as a magnet to hold it in place. Its movements are similar to those of an actuator.
BRIEF DESCRIPTION OF THE INVENTION
This invention addresses the above and other related needs with a resilient retainer structure and system which is reformed-in-place, i.e., a production-quality retainer with its tolerance variations is inserted into a system that can have significant tolerance variations, and is reformed-in-place to a new configuration which takes up small or large tolerance clearances as needed and then exerts a retentive force that is substantially independent of the tolerance take-up, and that provides essentially all of the force available with the yield strength of the retainer structure.
According to this invention, the retention spring is initially formed into a bow or a wave-shaped structure, whose extremities are short of their ultimately-intended working length. This enables rapid and easy placement in what will be its final working position. Then with special in-place re-forming tools and techniques, the ends of the "bow" or "wave" form retention springs are extended first adaptively to take up assembly clearance and tolerance variations, and then reformed further to "load" it in place. Limited intermediate sections of the retention spring are then permanently re-worked and reformed at apex points above the line between the working contacts at ends of the arms of the spring. This final re-working is limited to a relatively small portion of the spring's free length. In this limited area or areas the metal is permanently bent in a direction tending to open the bow curvature and thus to increase the intrinsic length of the spring and the bow-end forces against the next assemblies.
In effect, the spring is first only partially fabricated. It is made to an assembly length appreciably shorter than its working length. Then it is loosely assembled with the other parts, and reconfigured and loaded in place by the above methods. This reduces to insignificance the classical "spring-back" effects which tend to prohibit effective in-place loading of resilient members.
Large tolerances take-up capabilities are inherent in the reform techniques of this invention, and they can be further extended in preferred embodiments. The apex reforming technique itself can take up tolerances which are large in relation to the small working deflection lengths common in the comparatively short, stiff compression springs that are usually employed for assembly retention. Beyond this, curved or "wave" type segments at the ends of the spring can be configured so as to be compressed, and take a permanent set during the in-place, re-form operation, with the bow as a whole then taking its load-set during the final apex re-form process.
A preferred method for conveniently and uniformly taking up very large assembly tolerance variations is to curve the ends of the retainer arms to promote metal curling as the arms are extended during an initial compression of the apex and spreading of the arms of the retainer. During this initial reforming and spreading of the loosely assembled bow or wave spring the precurled ends of the spring slide on adjacent surfaces, and then engage the next articles at restraint angles which facilitate further curling of the ends in place, until the apex of the bow structure is deflected to its approximate working height--just prior to the final function of reconfiguration loading by local reforming, as previously described.
The above and other features of this invention will be fully understood from the following detailed description and the accompanying drawings, in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a cross section of the presently preferred embodiment of the invention taken at line 1--1 in FIG. 2;
FIG. 2 is a cross section taken at line 2--2 in FIG. 1;
FIGS. 3, 4 and 5 are cross sections similar to FIG. 2 showing sequential steps in the installation of the detent;
FIG. 6 is an end view showing another embodiment of the invention;
FIG. 7 is a bottom view of the presently preferred embodiment of the invention;
FIG. 8 is a top view of the presently preferred embodiment of the invention;
FIG. 9 is a fragmentary view taken at line 9--9 in FIG. 6;
FIG. 10 is a side view of the initial shape of the retention spring of FIGS. 6 and 9;
FIG. 11 is a cross-section taken at line 11--11 in FIG. 10;
FIG. 12 is a view similar to FIG. 9 showing a variation thereof;
FIGS. 13 and 14 show variations of basic unreformed retention spring shapes;
FIGS. 15 and 16 show two sequential steps accomplished by preferred tooling;
FIG. 17 is a fragmentary axial cross-section showing optical detents; and
FIG. 18 is a fragmentary transverse cross-section showing other optional detents.
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 shows a motor housing 10 which constitutes an important use for the instant invention. Such a housing includes a steel motor ring 11 which may be formed as a seamless tubing, or as a tubing formed with a seam. It has an outer wall 12, an inner wall 13, and a central axis 14. The inner wall is circularly curved.
It is customary for these motor rings to have attached to them a pair of permanent magnets 15, 16. Usually these are ceramic. The magnets have an inner surface 17 and an outer surface 18 whose curvature is the same as the inner wall, both being centered on the axis. The magnets include abutment surfaces 19, 20, 21, 22, one pair on each magnet. One face of each magnet faces another face on the other magnet. One of the objects of this invention is firmly to hold the permanent magnets in place against inner wall 13 so they do not slide along it or fall away from it. It is to be remembered that ceramic magnets are often quite brittle, and it is necessary that forces exerted on them not be exerted in such a manner or at such intensities as are likely to cause fracture of the magnet.
A retention spring 25 according to this invention is provided for holding the magnets in place. Magnets are given as an example of a use of this invention, and not as a limitation on the utility of invention. The initial, unreformed shape is best shown in FIGS. 3, 7 and 8. The retention spring is made of a metal such as carbon steel which has classic elastic stress-strain properties at lesser stresses, and an elastic limit above which permanent deformation occurs when greater stress is applied. This is to say that it inherently has a substantial spring-loaded capacity, and also that it can be permanently deformed.
The retention spring includes a pair of arm 26, 27 (FIG. 3) joined by an integral central apex or bight 28 which comprises a bend between the arms, thereby forming a dihedral angle between them. A convenient, and the presently-preferred, shape of the arms between their connecting bight and the points of contact with the next assembly, for example with the magnets and with the inside wall of the ring, is a substantially straight segment. In many preferred applications, at the free ends (the ends most distant from the apex or bight) both of the arms have a curvilinear surface 29, 30, respectively.
Surfaces 29 and 30 are formed as a curl in the metal. The metal is preferably slotted by slots 31, 32 to form a plurality of fingers 33, 34. These slots and fingers serve to distribute the pressure against the hard and potentially uneven surfaces of the magnet. However, the slots and fingers are optional depending on the unit forces to be applied by the curvilinear surface.
Significant design and construction features at the ends of the detent arms (whether they curl up or down, whether instead of curling during installation they are configured to bend to take up tolerance variations, whether they are simple arm extensions bowed into the magnet surfaces, and/or whether, and if so how the ends are slotted to adapt to uneven surfaces) are all pragmatic matters and will be determined by normal design and tests for optimum performance in each application. Persons skilled in the art will have no difficulty in designing correct configurations and dimensions for their individual installations. Suitable dimensions and specifications for a typical retainer spring to install in an inner wall with a diameter about 27/8" diameter, permanent magnets about 3/8" thick and spaced apart at their ends by approximately 1" to 1 3/16" at their inner surfaces are as follows: stock thickness 0.030"; stock width 11/4"; spring height preformed 0.55"; spring height final formed (reformed) 0.25"; spring length preformed 0.95"; spring length final formed: without restraints 1 1/4"; with restraints 1" to 13/16". A suitable material is reformable spring steel.
The installation of this device requires permanent deformation of the body in such a way as to increase the spacing apart of the outer ends of the arms absent restraint ("intrinsic length"). Of course, the abutment surfaces are normally essentially immovable and therefore they do constitute a restraint.
One of the problems of spring retainers is that a high retention force requires a stiff, high-rate spring which is very sensitive to dimensional tolerances. In order for such a spring to exert a suitable separative force, it ordinarily must itself be compressed and allowed to spring back against the abutment surfaces. Also, the effective spring force is quite sensitive to the spacing between the abutment faces and to the accuracy of the dimensions of the spring itself. It should also be remembered that in permanent magnet motor assemblies an increase of spacing between one pair of adjacent abutment faces decreases the spacing between the other pair, so that one spring might be installed too tightly and another one too loosely. An advantage of this invention is that it enables the springs to be formed in place and stressed correctly in accordance with the actual existing, not a theoretical, spacing between the abutment faces.
The magnets are installed while holding them as closely to a symmetrical installation as is reasonably possible along with the use of high rate assembly tooling. A pair of lower anvils 40, 41 are located axially along the inner wall, and have forming surfaces 42, 43, respectively, which are flat (FIGS. 3-5) or slightly concave (see FIGS. 15 and 16). A pair of upper anvils 44, 45 are provided to move radially as shown by arrows 46 in FIG. 4, and preferably will have a convex surface. The terms "upper" and "lower" for convenience relate only to the side of the spring the respective anvil is placed on. The relationship to the vertical is not material.
A retention spring is placed between each of the facing abutment surfaces, and it will be noted that there can be, and usually there will be, a loose fit. The retention spring need not be compressed in order to set it between the abutment faces. Most conveniently, it will be inserted from the end, and need not clear inner corners 47, 48. In any event, it can form a loose fit relative to its adjacent abutment faces, thereby illustrating the freedom of this device from close tolerance constraints in the course of assembly.
In the next step of installation, the anvils are moved to contact the center of the retainer apex or bight, and this forces the fingers outwardly and sidewardly so as to contact both the inner wall of the ring and the respective abutment face. This takes up the tolerances in the system. The anvils continue to move the retainer apexes toward, but not beyond lines drawn between the points of contact with the abutment surfaces. This further movement causes the arms to bow, i.e., bend convexly away from the wall of the ring. This bowing deformation is at least partially temporary because if released there would be spring back even though some permanent deformation also results. Thus, even though the retention spring has at this stage been deflected to take up tolerances and apply load to the magnets and ring assembly, if it were released there would be substantial spring back, and an optimally reliable assembly would not be produced. To avoid spring back and to assure maximum retention forces on the magnet assembly, the final spring reforming stage is a permanent re-working of a localized region or regions which has the effect of reversing or opening the bow curvature and thus increasing the lateral spring load.
The initial spread of the arms, and the bowing action are shown in FIG. 4. Because of the properties of the metal, the angular bight or apex in this configuration does not simply open like a book. Instead, the arms spread and bow slightly and after taking up clearances, the fingers yield as necessary to relieve excessive localized forces on the abutting surfaces. A "peak" 28a, which is exaggerated in FIG. 4 remains. Even if not so pronounced, it still is a raised, rounded local region. When anvils 44 and 45 finally close they rework and permanently change the curvature of the bight in the localized area, so as to cause the dihedral angle between the arms to increase, thus further bowing the balance of the length of arms- causing bending stresses at least close to, and preferably beyond the yield point. The increases in the bow stresses of the arms increases the separative forces at the ends of the arms.
This reformation in place has occurred after the retention spring has taken up the tolerances and received an initial bowing spring tension. However variable these may have been, there is enough movement left as the consequence of the final permanent deformation to provide in a given retainer structure close to maximum separative forces irrespective of relatively large variations in assembled length. Spring-back unloading is slight because it is limited to the small portion of the bow retainer which is reworked between anvils 44 and 45. Thus, a reliable and suitable predictable spring load is generated in the retention spring after it is placed in its working position.
The rather easier bending of the fingers permits readier adaption of shape of the permanently deformed detent over a broader range of tolerances of parts and their installation. it is evident that the force exerted by the inner anvil has caused a permanent deformation by virtue of having stressed the metal at a stress level in excess of its elastic limit. FIG. 4 illustrates that the geometry of the anvil surfaces and of the bight is such that a change of shape in the sense of changing the bend can readily occur.
The anvils are now separated and the tool assembly slid out--the slight spring-back of the retention spring permitting ready removal of the tools.
It will be observed that this installation has been caused by a simple application of force between upper and lower anvils creating a retention system which is entirely related to each specific installation rather than to theoretical dimensions.
There are important possible variations to the simplest embodiment shown in FIGS. 1-5, 7 and 8. For example, a retention spring 70 is shown in FIG. 13 which has all of the features and the same general construction as retention spring 25. It differs in that its bight 71 has a rounded apex 72 which makes more pronounced the spreading and bowing of the arms 73, 74 when the apex is flattened against the anvil.
FIG. 14 shows a retention spring 80 whose bight 81 is more complex. It has a dimension of width, and includes two apexes 82, 83 similar to apex 72. This construction is useful when longer separations are to be spanned. Two sets of anvils are used, one for each of the apexes. Apart from the plurality of apexes, and differences in dimensions retention spring 80 is in all respects similar to spring 25.
FIGS. 15 and 16 show preferred tooling. A moving upper anvil 90 and fixed lower anvil 91 are provided as before. However, anvil 90 has a curved nose 92, and anvil 91 has a concave forming face 93 with a recessed central portion 94 and a peak 95, 96 on each side of it. FIG. 15 shows the tooling at the end of the first step- it has expanded the retention spring to take up the tolerances and made the initial bowing.
FIG. 16 shows the final step, and here the moving anvil has travelled the full distance and formed in a limited length of the bow a concave shape 97 at the bight. Thus, the central region has had an even more profound change of curvature to spread the arms than if the lower anvil were flat.
Centering notches 99 are optionally formed in the edges of the bight. These or other provisions such as a single hole can be engaged by tooling to hold the spring centered during the setting so as not to drift off excessively to one side or the other.
FIGS. 6 and 9-12 illustrate that the bight of the retainer spring need not extend axially along the wall of the ring, but instead can be normal to it. Otherwise stated, a plane cut normally through the bight and both arms lies along the wall, rather than normal to the wall.
In FIG. 6, two retainer springs 100, 101 are shown interposed between magnets 102, 103, bearing against abutment faces 104, 105, 106 and 107. They also bear against the inside wall 108 of the steel ring 109. The detailed construction of these identical retainer springs is best shown in FIGS. 9-11.
In FIG. 9, spring 100 is shown with a central bight 110 and two arms 111, 111a. This spring is formed from wire or rod. As best shown in FIG. 11, it has generally rounded corners, and an outer straight face 112 (contact surface) that bears against the abutment surface. The initial shape of the spring is shown in FIG. 10, where the bight can be initially flat or rounded upward as previously shown. A flat bight is somewhat more advantageous, because when the anvils are pressed against it, it will tend to remain centered, rather than to drift to one side. However, a somewhat rounded or even peaked bight will perform satisfactorily. The legs are spread apart by a nominal distance which will enable the spring to be placed between the abutment surfaces with ease. Then the retainer spring is reworked between anvils in a limited portion of its working length, as previously described, to reverse the bow curvature and cause the arms to spread apart, take up the tolerances, and stress-load the bow. Tooling similar to that shown in FIGS. 15 and 16 can be used. the most advantageous technique is to form a reverse curve 113 in the bight as shown. Alternatively, the bight could have been made with an initial convex shape, and been flattened when the spring was reformed in place.
FIG. 12 shows a retention spring which is essentially a combination of two of the springs shown in FIGS. 9-11. It has a pair of bights 121, 122, and each bight connects a pair of arms as before. However, two of the arms are connected. The setting of this spring is identical to that of the embodiment of FIG. 9, except that two sets of tooling are used simultaneously.
FIG. 17 shows additional means to secure the assembly against unusual shock loads which might be experienced in shipping or abnormal use. A tube 200 within inner wall 201 receives a pair of magnets 202, 203 as in the other embodiments. The tube has a central axis 204. A retention spring 205 according to any of the embodiments is installed between two magnets. Detents to restrict any vibrating or shock displacements of magnets, for example detents 206, 207 may be located on the inside wall of the tube. These may be metal, and may constitute raised stud-like structures, which can be located where either or both of the ends of the magnets are to be located. Any desired number of detents can be provided, and if preferred, the detents could instead be ring-like structures.
For some installations, it is sufficient to use only one retention spring. An example is shown in FIG. 18, where tube 210 with an inner wall 211 has magnets 212, 213 held in it by means of retention spring 214. Spring 214 can be according to any of the embodiments disclosed herein. The abutting surfaces 215, 216 away from spring 214 must, of course, be restrained. A spacer (not shown) could be placed in abutment with these surfaces, or instead detents 217, 218 may be formed on the inner wall to be borne against by the magnets. As in FIG. 17, the detents could be created by deformation of the metal by a force exerted on the outer wall of the tube.
In summary, in all embodiments, a retention spring is made from reformable resilient metal into a bow or a wave-type structure with arms at each end to contact and oppose abutment surfaces on articles to be retained. The spring has a bight with one or more apex portions at a location off of (above) the load contact points, and also above the ultimately reformed assembly height of the retention spring.
The installation procedure involves three sequential operations:
a. Reducing the height of the spring with the concomitant extension of the arms to take up assembly clearances. This may be accomplished initially by causing the arms to slide along a surface such as the inside wall of the ring, or solely by spreading the arms by reversing the curvature in a limited bight or apex portion of the spring.
b. Further reducing the height and/or reversing the bight curvature to provide a bowing deformation (which may be permanent) to spring-load the arms against the abutment surfaces. This is a continuation of step a, above, and can result in random bending of the arms, more closely controlled bending if the geometry is designed for it, or a curling of portions designed for the purpose, such as the fingers in FIGS. 1-5.
c. The final reworking of a limited apex region, which permanently deforms that region to change its curvature, and increase the bow curvature and stress in the arms.
It is further to be observed that, instead of retaining two articles with the use of the two retainer spring, each of the retainer springs bearing against two articles, one of the abutment surfaces could be on fixed structure instead and only one article retained. Furthermore, permanent detents can be used in lieu of one of the retention springs.
The term "intrinsic length" is sometimes used herein. This term is meant to describe what would be the length of the retention spring (i.e., the spacing between its contact points) absent restraint. This is not the first extension where the spring is deflected to take up the assembly clearances. Instead it is the consequence of the further bowing of the arms, and of the permanent reformation in the limited area in the bight. This intrinsic increase in length, is never actually realized by the spring retainer, because its extension is resisted by the abutment surfaces, causing the arms to become bowed and to store energy. Thus when the reworking forces are removed, the spring-back energy looses are limited to that relatively small portion of its working length which was reworked to reverse the bow curvature. The retainer is quickly and efficiently set in place with its ultimate configuration and maximum loading irrespective of varying assembly tolerences.
This invention is not to be limited by the embodiments shown in the drawings and described in the description, which are given by way of example and not of limitation, but only in accordance with the scope of the appended claims. | Secure and rapid assembly of magnets or other articles in tubular or other-shaped housings is achieved with bow type compression retainers which are made from reformable spring metal, and are initially formed shorter and higher than their ultimate working dimensions to permit loose or easy manual or automatic assembly in their final working location, after which the retainers can be reformed in place to a reduced height and extended length so as to take up any clearance and to place an initial load on abutting faces of the article to be secured. Then the bow shaped retainer is finally reworked in a comparatively small portion of its length, and in a direction which tends to change the natural curvature and extend the intrinsic unloaded length of the restrained bow, thus off-setting "spring back" type load losses characteristic of normal spring forming, and assuring maximum spring retention forces irrespective of large assembly tolerances and high spring rates. Provisions for metal curling or bending near the ends of the retainer can further extend tolerance take-up capabilities; and several preferred means are shown for accomplishing the final curvature-reversal loading of the retainers. | 5 |
BACKGROUND
[0001] Turbine engines, and particularly gas or combustion turbine engines, are rotary engines that extract energy from a flow of combusted gases passing through the engine onto a multitude of rotating turbine blades. Typically a fan section is utilized to take in ambient air and direct it to different components of the engine for extracting energy and cooling purposes. Some of the fan air is initially directed into the compressor stages, while other portions of the fan air continue through outlet guide vanes and can later be directed into the engine components as needed.
[0002] Gas turbine engines include offtakes in areas of the engine where air is extracted from high-velocity, swirling channels to the internal air system for cooling, sealing or heat management purposes. When the angle of redirection is 90° or higher louvers or other aerodynamic shapes are required to turn the flow effectively. The louvers are typically cascades of equal length, shape and camber angle.
BRIEF DESCRIPTION
[0003] In one aspect, embodiments of relate to gas turbine engine comprising an annular fan exhaust section, an engine core at least partially located within the fan exhaust section, a cooling air offtake located in the engine core and having an inlet, a louver located at the inlet and having at least two different size airfoils in spaced axial arrangement.
[0004] In another aspect, embodiments relate to a louver assembly for an off take of a gas turbine engine comprising at least four airfoils in axial arrangement, with none of the airfoils are of the same size.
BRIEF DESCRIPTION OF THE DRAWINGS
[0005] In the drawings:
[0006] FIG. 1 is a schematic cross-sectional diagram of a gas turbine engine for an aircraft.
[0007] FIG. 2 is an enlarged view of a fan exhaust section of the gas turbine engine of FIG. 1 .
[0008] FIG. 3 is an enlarged view of an inlet with a louver having multiple airfoils for a cooling offtake duct for the gas turbine engine of FIG. 1 .
[0009] FIG. 4A is a flow diagram of a conventional louver assembly.
[0010] FIG. 4B is a flow diagram of an embodiment of the proposed louver assembly.
DETAILED DESCRIPTION
[0011] The described embodiments of the present invention are directed to a gas turbine engine have a louver to redirect fan air. For purposes of illustration, embodiments of the present invention will be described with respect to the turbine for an aircraft gas turbine engine. It will be understood, however, that the embodiments of the invention are not so limited and may have general applicability within an engine, including compressors, as well as in non-aircraft applications, such as other mobile applications and non-mobile industrial, commercial, and residential applications.
[0012] As used herein, the term “forward” or “upstream” refers to moving in a direction toward the engine inlet, or a component being relatively closer to the engine inlet as compared to another component. The term “aft” or “downstream” used in conjunction with “forward” or “upstream” refers to a direction toward the rear or outlet of the engine relative to the engine centerline.
[0013] Additionally, as used herein, the terms “radial” or “radially” refer to a dimension extending between a center longitudinal axis of the engine and an outer engine circumference.
[0014] All directional references (e.g., radial, axial, proximal, distal, upper, lower, upward, downward, left, right, lateral, front, back, top, bottom, above, below, vertical, horizontal, clockwise, counterclockwise, upstream, downstream, aft, etc.) are only used for identification purposes to aid the reader's understanding of the present embodiments, and do not create limitations, particularly as to the position, orientation, or use of the embodiments. Connection references (e.g., attached, coupled, connected, and joined) are to be construed broadly and can include intermediate members between a collection of elements and relative movement between elements unless otherwise indicated. As such, connection references do not necessarily infer that two elements are directly connected and in fixed relation to one another. The exemplary drawings are for purposes of illustration only and the dimensions, positions, order and relative sizes reflected in the drawings attached hereto can vary.
[0015] FIG. 1 is a schematic cross-sectional diagram of a gas turbine engine 10 for an aircraft. The engine 10 has a generally longitudinally extending axis or centerline 12 extending forward 14 to aft 16 . The engine 10 includes, in downstream serial flow relationship, a fan section 18 including a fan 20 , a compressor section 22 including a booster or low pressure (LP) compressor 24 and a high pressure (HP) compressor 26 , a combustion section 28 including a combustor 30 , a turbine section 32 including a HP turbine 34 , and a LP turbine 36 , and an exhaust section 38 .
[0016] The fan section 18 includes a fan casing 40 surrounding the fan 20 . The fan 20 includes a plurality of fan blades 42 disposed radially about the centerline 12 . The fan casing 40 can also surround at least a portion of the fan exhaust section 41 . The HP compressor 26 , the combustor 30 , and the HP turbine 34 form a core 44 of the engine 10 , which generates combustion gases. The core 44 is surrounded by core casing 46 , which can be coupled with the fan casing 40 , so that the core 44 is at least partially located within the fan exhaust section 41 .
[0017] A HP shaft or spool 48 disposed coaxially about the centerline 12 of the engine 10 drivingly connects the HP turbine 34 to the HP compressor 26 . A LP shaft or spool 50 , which is disposed coaxially about the centerline 12 of the engine 10 within the larger diameter annular HP spool 48 , drivingly connects the LP turbine 36 to the LP compressor 24 and fan 20 .
[0018] The LP compressor 24 and the HP compressor 26 respectively include a plurality of compressor stages 52 , 54 , in which a set of compressor blades 56 , 58 rotate relative to a corresponding set of static compressor vanes 60 , 62 (also called a nozzle) to compress or pressurize the stream of fluid passing through the stage. In a single compressor stage 52 , 54 , multiple compressor blades 56 , 58 can be provided in a ring and can extend radially outwardly relative to the centerline 12 , from a blade platform to a blade tip, while the corresponding static compressor vanes 60 , 62 are positioned upstream of and adjacent to the rotating blades 56 , 58 . It is noted that the number of blades, vanes, and compressor stages shown in FIG. 1 were selected for illustrative purposes only, and that other numbers are possible.
[0019] The blades 56 , 58 for a stage of the compressor can be mounted to a disk 59 , which is mounted to the corresponding one of the HP and LP spools 48 , 50 , with each stage having its own disk 59 , 61 . The vanes 60 , 62 for a stage of the compressor can be mounted to the core casing 46 in a circumferential arrangement.
[0020] The HP turbine 34 and the LP turbine 36 respectively include a plurality of turbine stages 64 , 66 , in which a set of turbine blades 68 , 70 are rotated relative to a corresponding set of static turbine vanes 72 , 74 (also called a nozzle) to extract energy from the stream of fluid passing through the stage. In a single turbine stage 64 , 66 , multiple turbine vanes 72 , 74 can be provided in a ring and can extend radially outwardly relative to the centerline 12 , while the corresponding rotating blades 68 , 70 are positioned downstream of and adjacent to the static turbine vanes 72 , 74 and can also extend radially outwardly relative to the centerline 12 , from a blade platform to a blade tip. It is noted that the number of blades, vanes, and turbine stages shown in FIG. 1 were selected for illustrative purposes only, and that other numbers are possible.
[0021] The blades 68 , 70 for a stage of the turbine can be mounted to a disk 71 , which is mounted to the corresponding one of the HP and LP spools 48 , 50 , with each stage having its own disk 71 , 73 . The vanes 72 , 74 for a stage of the compressor can be mounted to the core casing 46 in a circumferential arrangement.
[0022] The portions of the engine 10 mounted to and rotating with either or both of the spools 48 , 50 are also referred to individually or collectively as a rotor 53 . The stationary portions of the engine 10 including portions mounted to the core casing 46 are also referred to individually or collectively as a stator 63 .
[0023] In operation, the airflow exiting the fan section 18 is split such that a portion of the airflow is channeled into the LP compressor 24 , which then supplies pressurized ambient air 76 to the HP compressor 26 , which further pressurizes the ambient air. The pressurized air 76 from the HP compressor 26 is mixed with fuel in the combustor 30 and ignited, thereby generating combustion gases. Some work is extracted from these gases by the HP turbine 34 , which drives the HP compressor 26 . The combustion gases are discharged into the LP turbine 36 , which extracts additional work to drive the LP compressor 24 , and the exhaust gas is ultimately discharged from the engine 10 via the exhaust section 38 . The driving of the LP turbine 36 drives the LP spool 50 to rotate the fan 20 and the LP compressor 24 .
[0024] A remaining portion of the airflow 78 bypasses the LP compressor 24 travelling through the fan exhaust section 41 and exiting the engine assembly 10 through a stationary vane row, and more particularly an outlet guide vane assembly 80 , comprising a plurality of airfoil guide vanes 82 . More specifically, a circumferential row of radially extending airfoil guide vanes 82 are utilized adjacent the fan section 18 to exert some directional control of the airflow 78 . Upon exiting the fan exhaust section 41 , the airflow 78 can be redirected using a cooling air offtake 84 for additional cooling of the engine core 44 and turbine section 32 .
[0025] Some of the ambient air supplied by the fan 20 can bypass the engine core 44 and be used for cooling of portions, especially hot portions, of the engine 10 , and/or used to cool or power other aspects of the aircraft. In the context of a turbine engine, the hot portions of the engine are normally the combustor 30 and components downstream of the combustor 30 , especially the turbine section 32 , with the HP turbine 34 being the hottest portion as it is directly downstream of the combustion section 28 . Other sources of cooling fluid can be, but is not limited to, fluid discharged from the LP compressor 24 or the HP compressor 26 . This fluid can be bleed air 77 which can include air drawn from the LP or HP compressors 24 , 26 that bypasses the combustor 30 as cooling sources for the turbine section 32 . This is a common engine configuration, not meant to be limiting.
[0026] FIG. 2 is an enlarged view of the area near the fan exhaust section 41 . The cooling air offtake 84 comprises a duct 86 having walls 88 that turn through nearly 90° from a primarily radial orientation to a primarily axial orientation. The cooling air offtake 84 includes an inlet 90 located downstream of the outlet guide vane assembly 80 . The inlet 90 includes a louver assembly 92 having a louver 93 comprising at least two different size airfoils 94 , 96 . While illustrated at a location downstream of the fan exhaust section 41 , the offtake 84 can be located at any appropriate location throughout the engine.
[0027] In an exemplary embodiment illustrated in FIG. 3 the louver assembly 92 includes four airfoils 94 , 96 , 98 , 100 spaced in an axial arrangement. The inlet 90 has a leading edge 85 with a rounded lip and a trailing edge 87 having a chamfer angle β of at least 20°, but not to exceed 30° measuring from the duct wall 88 towards the trailing edge 87 axially upstream. This feature will allow for higher pressure air bleed and moving the impingement point aft. An excessive angle will result in undesired pressure losses.
[0028] The geometry of airfoil 96 , which will be referred to as the primary airfoil 96 , is outlined in FIG. 4 described by a chord length C having a length defined as a line from a leading edge 108 to a trailing edge 110 and a height H having a length defined as a line from a radial maximum 112 to a radial minimum 114 relative to the engine centerline. Each airfoil is also described by an angle of attack α measured from a local relative wind direction 116 to a continuous line along the chord length C. For illustrative purposes the dimensions for an initial, third, and fourth airfoil 94 , 98 , 100 will be represented by subscripts 1 , 2 , and 3 respectively.
[0029] The primary airfoil 96 is geometrically larger, both with respect to the chord length C and the height H, than the other three airfoils 94 , 98 , 100 . The maximum height H of the primary airfoil 94 is at least 2 times larger than the maximum height H 1 of the initial airfoil 94 . The chord length C is at least 2.5 times larger than the chord length C 1 . The axial arrangement of the airfoils comprises a geometry partially defined by a chord length relationship as follows:
[0000] C>C 3 >C 1 ≧C 4
[0030] The spaced axial arrangement includes the initial airfoil 94 nearest the leading edge 85 of the inlet 90 , after which the primary airfoil 96 is located downstream of the initial airfoil 94 , followed in the downstream direction by the third and fourth airfoils 98 , 100 . The third and fourth airfoils 98 , 100 are spaced equivalently so that the distance between the duct wall 88 and the fourth airfoil 100 is nearly the same as the distance between the third and fourth airfoils 98 , 100 . This spacing prevents flow separation between airfoils whilst keeping a Mach number high (See FIGS. 4A and 4B )
[0031] The angle of attack a for the third and fourth airfoils 98 , 100 is different than the angle of attack a for the first and second airfoil 94 , 96 . In an exemplary embodiment the angle of attack a for the third and fourth airfoils 98 , 100 is greater than that of the first and second airfoil 94 , 96 .
[0032] In an exemplary embodiment, the trailing edges 110 of the third and fourth airfoils 98 , 100 terminate in a line L connecting the trailing edge 110 of the primary airfoil 96 to a point 118 downstream of a trailing edge 87 of the inlet 90 . This geometry causes corresponding chord lengths C 3 , C 4 for the third and fourth airfoil 96 , 98 become consecutively shorter. This relationship manages to turn effectively the flow whilst reducing any friction losses due to flow contact with the airfoil surface.
[0033] The overall benefit of the current embodiments is seen by the comparison of FIG. 4A , showing a contemporary louver assembly with equal sized airfoils, with substantially the same angle of attack and equal spacing, as compared to the embodiment of FIGS. 2-3 . For the conventional louver assembly the flow direction is changed by guiding the airflow using a louver 122 having similar shaped airfoils 124 as depicted in FIG. 4A . This design can cause airflow separation 126 which is undesirable for effective airflow movement. Increasing the size of the primary airfoil 94 so that the louver assembly 92 comprises at least two different size airfoils 94 , 96 where the second 96 is geometrically larger than the first 94 . This geometry differentiation causes an acceleration 128 of the flow depicted in FIG. 4B allowing for a total engine pressure P t increase.
[0034] Each of the airfoils 94 , 96 , 98 , 100 in the louver assembly 92 is designed with a purpose, ensuring the effective use of the individual aerodynamic geometry. The initial airfoil 94 is configured to stabilize a boundary layer 130 and contain recirculation 132 in the duct 86 . With a conventional louver assembly 120 the boundary layer 131 is too thick and will induce separation, wherein as seen in FIG. 4B , the boundary layer 130 by both the initial airfoil 94 and primary airfoil 96 is well defined. The primary airfoil 96 is configured to accelerate 128 the flow to maximum speed 134 without flow separation. The third and fourth airfoils 98 , 100 are configured to guide the flow from downstream of the primary airfoil 96 in order to prevent separation.
[0035] Thorough CFD (Computational Fluid Dynamics) analyses has been conducted and supports the benefit of the louver assembly 92 as compared to conventional louver assemblies 120 . 2D optimization backed up with a 3D analysis has been carried out with tabulated results following. The pressure recovery is maximized whether considering an area from the fan exhaust section 41 to the HP turbine 34 or from the fan exhaust section 41 to the LP turbine 36 both of which enable a reduction in bled flow. The following table compares a first engine recovery ratio to a second engine recovery ratio where the second engine recovery ration includes the louver assembly 92 in place and the pressure recovery is at least 0.30. The goal is to maintain the highest total pressure (P t ) as possible so as to best move air through the duct to the turbine sections.
[0000]
Total
Static
Pressure
Pressure
Total
Recovery = (Pt − P s13 )/
Recov-
(Stage 13)
(Stage 13)
Pressure
(P t13 − P s13 )
ery
P t13
P s13
P t
One Engine with conventional
0.131
8.07
6.82
6.99
louver design
Second Engine with proposed
0.362
8.369
7.097
7.557
louver assembly through the
HP turbine
Second Engine with proposed
0.349
8.369
7.097
7.541
louver assembly through the
LP turbine
[0036] Benefits to increasing the pressure recovery and reducing the mass flow include allowing for the duct flow to be reduced while maintain power. As the room for designing pipes is typically constrained, the introduction of this approach enables that duct pipes to be designed with more flexibility.
[0037] It should be appreciated that application of the disclosed design is not limited to turbine engines with fan and booster sections, but is applicable to turbojets and turbo engines as well.
[0038] This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any incorporated methods. The patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims. | An apparatus and method are disclosed for a gas turbine engine including an offtake located within the air flow of the engine. The offtake has an inlet and a louver covering the inlet. The louver has multiple airfoils arranged to direct the air flow into the inlet of the offtake. | 5 |
BACKGROUND OF THE INVENTION
The present invention relates to a novel silyl thioalkene compound having a silicon atom and a sulfur atom in the molecule, which is useful as an intermediate in the synthesis of various kinds of organic compounds, as well as to a method for the preparation of the compound.
A silyl thioalkene compound is a compound having a silicon atom and a sulfur atom in the molecule so that the compound is useful in the synthetic preparation of an organic compound having a sulfur atom by undertaking a position-specific or stereospecific coupling reaction between the compound and an organic halogen compound in the presence of a catalyst readily to form a carbon-carbon linkage and in the preparation of a diol or enol ether compound having a sulfur atom in the molecule by undertaking the so-called osmium oxidation. Accordingly, silyl thioalkene compounds are expected to be useful as a starting material or an intermediate compound in the synthesis of various kinds of organic compounds as a medicine or as an agricultural chemical.
Several methods are proposed in the prior art for the synthetic preparation of certain silyl thioalkene compounds including a method by the photochemical reaction between a silylalkyne compound and a thiol compound under irradiation with light in the presence of a radical initiator and a method by the coupling reaction between a silylalkenyl halide compound and stannyl sulfide in the presence of a catalyst. These methods, however, are industrially not advantageous because the silyl group-containing compound as the starting material cannot be obtained without difficulties. Accordingly, it is eagerly desired to obtain a novel silyl thioalkene compound capable of being synthesized directly from a hydrocarbon compound.
SUMMARY OF THE INVENTION
The present invention accordingly has an object, in view of the above described situations in the prior art, to provide a novel silyl thioalkene compound useful as a synthesis reagent in the field of fine chemicals by an industrially advantageous efficient method by using readily available starting materials.
Thus, the present invention provides, firstly, a silyl thioalkene compound represented by the general formula
R(--CSAr═CHSiX.sub.3).sub.n, (I)
in which the subscript n is 1 or 2, R is a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group, when n is 1, or a divalent hydrocarbon group, when n is 2, Ar is an unsubstituted or nucleus-substituted monovalent aromatic hydrocarbon group and X is a halogen atom or a hydrocarbyloxy group.
The above defined silyl thioalkene compound represented by the general formula (I), in which the group X is a halogen atom, can be prepared by the following methods developed by the inventors.
Firstly, the silyl thioalkene compound of the general formula (I), in which the group X is a halogen atom, denoted by X 1 hereinafter, i.e. halogenosilyl thioalkene compound, is prepared by the method, referred to as the first method hereinafter, which comprises the step of:
reacting an alkyne compound represented by the general formula
R(--C.tbd.CH).sub.n, (II)
in which the subscript n is 1 or 2 and R is a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group, when n is 1, or a divalent hydrocarbon group, when n is 2, with a silyl sulfide compound represented by the general formula
ArS--SiX.sup.1.sub.3, (III)
in which Ar is an unsubstituted or nucleus-substituted monovalent aromatic hydrocarbon group and X 1 is a halogen atom, in the presence of a platinum complex compound as a catalyst.
Alternatively, the silyl thioalkene compound of the general formula (I), in which the group X is a halogen atom, denoted by X 1 , is prepared by the method, referred to as the second method hereinafter, which comprises the step of:
reacting a disulfide compound represented by the general formula
ArS--SAr, (IV)
in which Ar has the same meaning as defined above, with a hexahalogenodisilane compound represented by the general formula
X.sup.1.sub.3 Si--SiX.sup.1.sub.3, (V)
in which X 1 has the same meaning as defined above, and an alkyne compound or an alkadiyne compound represented by the general formula
R(--C.tbd.CH).sub.n, (VI)
in which R and n each have the same meaning as defined above, in the presence of a platinum complex compound as a catalyst.
Further, the silyl thioalkene compound of the general formula (I), in which the group X is an unsubstituted or substituted monovalent hydrocarbon group, denoted by X 2 hereinafter, can be prepared by the method, referred to as the third method hereinafter, which comprises the step of:
reacting the halogenosilyl thioalkene compound obtained by the first or second method described above and represented by the general formula
R(--CSAr═CHSiX.sup.1.sub.3).sub.n, (VII)
in which each of the symbols has the same meaning as defined above, with a hydrocarbon carbonium ion-generating compound.
The silyl thioalkene compound of the general formula (I), in which the group X is a hydrocarbyloxy group, denoted by --OX 2 hereinafter, is prepared by the method, referred to as the fourth method hereinafter, which comprises the step of:
reacting the halogenosilyl thioalkene compound obtained by the first or second method described above and represented by the general formula (VII) given above with an alcohol compound represented by the general formula
X.sup.2 --OH, (VIII)
in which X 2 has the same meaning as defined above, in the presence of a dehydrohalogenating agent to effect a dehydrohalogenation reaction.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The silyl thioalkene compound of the present invention represented by the above given general formula (I) is a novel compound not known in the prior art or not described in any literatures although certain related compounds having methyl groups as the groups X in the general formula (I) are disclosed in Journal of the Chinese Chemical Society, volume 43 (1996), page 43, 53-59 and Tetrahedron Letters, volume 30 (1989), pages 2699-2702. When the subscript n in the general formula (I) is 1, the compound is represented by the general formula
R--CSAr═CHSiX.sub.3, (Ia)
in which R is a hydrogen atom or an unsubstituted or substituted monovalent hydrocarbon group and Ar and X each have the same meaning as defined above. When the subscript n in the general formula (I) is 2, the compound is a bis(silyl thioalkene) compound represented by the general formula
X.sub.3 Si--CH═CSAr--R--CSAr═CH--SiX.sub.3, (Ib)
in which R is a divalent hydrocarbon group and Ar and X each have the same meaning as defined above.
The monovalent hydrocarbon group denoted by R in the above given general formula (Ia) is exemplified by alkyl groups such as methyl, ethyl, propyl and butyl groups, alkenyl groups such as ethenyl, propenyl and butenyl groups, cycloalkyl groups such as cyclopentyl and cyclohexyl groups, cycloalkenyl groups such as cyclohexenyl group, aryl groups such as phenyl, tolyl, xylyl and naphthyl groups and aralkyl groups such as benzyl and phenethyl groups.
The monovalent hydrocarbon group denoted by R can be substituted by atoms or groups such as halogen atoms and alkoxy, amino, cyano, nitro, alkylcarbonyloxy and acyl groups. Particular examples of such a substituted monovalent hydrocarbon group include 2-chloroethyl, 3-chloropropyl, 4-bromobutyl, 2-methoxyethyl, 3-aminopropyl, 2-cyanoethyl, 3-cyanopropyl, 4-nitrobutyl, tribromodimethyl sulfonylbutyl, tert-butylcarbonyloxyethyl, 4-chlorophenyl and 4-acetylphenyl groups.
The unsubstituted or substituted monovalent aromatic hydrocarbon group denoted by Ar is exemplified by phenyl, 4-chlorophenyl, 4-bromophenyl and 4-methoxyphenyl groups.
The halogen atom denoted by X in the general formula (I) includes atoms of fluorine, chlorine, bromine and iodine. The monovalent hydrocarbon group denoted by X is exemplified by alkyl groups such as methyl, ethyl and propyl groups, cycloalkyl groups such as cyclopentyl and cyclohexyl groups, aryl groups such as phenyl and tolyl groups and aralkyl groups such as benzyl group. The hydrocarbyloxy group denoted by X is exemplified by methoxy, ethoxy, propoxy, cyclohexyloxy, phenoxy and benzyloxy groups.
When the subscript n is 2 to give the general formula (Ib), R is a divalent hydrocarbon group which is exemplified by alkylene groups such as methylene, tetramethylene and pentamethylene groups and arylene groups such as phenylene and naphthylene groups, optionally, substituted by functional groups. Ar and X in the general formula (Ib) can be exemplified by the same atoms and/or groups as those for the general formula (Ia).
The silyl thioalkene compound of the invention represented by the above given general formula (Ia) or (Ib) can be synthetically prepared by either one of the above described first to fourth methods.
In the first method, an alkyne compound or alkadiyne compound represented by the general formula (II) is reacted with the silyl sulfide compound represented by the general formula (III) to give the silyl thioalkene compound of the general formula (I) in which X is a halogen atom.
The alkyne compound represented by the general formula (II) is exemplified by acetylene, butyne, octyne, phenylacetylene, propargyl ether and cyclohexenylacetylene and the alkadiyne compound is exemplified by 1,4-pentadiyne, 1,8-nonadiyne and diethynyl benzene.
The silyl sulfide compound represented by the general formula (III) to be reacted with the alkyne or alkadiyne compound described above is exemplified by trichlorosilyl phenyl sulfide, tribromosilyl phenyl sulfide and trifluorosilyl phenyl sulfide.
In the second method, the above described alkyne or alkadiyne compound of the general formula (II) is reacted with the disulfide compound represented by the general formula (IV) and the hexahalogenodisilane compound represented by the general formula (V) in combination. The disulfide compound of the general formula (IV) is exemplified by diphenyl disulfide, bis(4-chlorophenyl) disulfide, bis(4-bromophenyl) disulfide and bis(4-methoxyphenyl) disulfide. The hexahalogenodisilane compound of the general formula (V) is exemplified by hexachlorodisilane, hexafluorodisilane and hexabromodisilane.
The platinum complex compound used as a catalyst in the reactions of the first and second methods of the invention is preferably a complex compound of platinum in a lower atomic valency or, in particular, a zero-valency platinum complex with tertiary phosphine or phosphite as the ligand, though not particularly limitative thereto. Alternatively, it is optional to use a precursor complex which can readily be converted in situ into a zero-valency platinum complex in the reaction mixture. Further, it is sometimes advantageous to admix the reaction mixture with an appropriate platinum compound without ligands and a tertiary phosphine or phosphite in combination resulting in formation in situ of a zero-valency platinum complex with the tertiary phosphine or tertiary phosphite as the ligand to serve as a catalyst. Various kinds of tertiary phosphines and phosphites can be used as the ligand in the platinum complex to exhibit high catalytic activity although those having excessively high electron donating activity are not always preferable in respect of obtaining a high reaction rate. Examples of preferable ligands include triphenylphosphine, tris(4-chlorophenyl)phosphine, tris(4-fluorophenyl)phosphine, tritolylphosphine, diphenylmethylphosphine, phenyldimethylphosphine, diphenylcyclohexylphosphine, phenyldicyclohexylphosphine, 1,4-bis(diphenylphosphino)butane, trimethyl phosphite and triphenyl phosphite, which can be introduced into the platinum complex either singly or as a combination of two kinds or more.
Some of the examples of other platinum complex compounds without tertiary phosphine or phosphite as the ligand include bis(1,5-cyclooctadiene)platinum and bis (dibenzylideneacetone)platinum. Examples of preferable phosphine- or phosphite-platinum complex compounds include tetrakis (triphenylphosphine)platinum, tris(triphenylphosphine)platinum and ethylenebis(triphenylphosphine)platinum. These platinum complex compounds can be used as the catalyst in the inventive method either singly or as a combination of two kinds or more according to need.
In practicing the first and second methods of the present invention, it is optional that the reaction mixture is diluted by the addition of an organic solvent, which is preferably a hydrocarbon solvent or an ether solvent. The amount of the platinum complex compound added to the reaction mixture as a catalyst is, though not particularly limitative within a range of the so-called catalytic amount, usually 20% by moles or smaller based on the amount of the alkyne or alkadiyne compound as the starting material.
While the reaction mixture in practicing the first and the second methods of the present invention is formed by mixing an alkyne compound or alkadiyne compound with a silyl sulfide compound or a combination of a disulfide compound and a hexahalogenodisilane compound, respectively, it is usually advantageous that the respective reactants are used in a stoichiometric proportion, although a small deviation from the stoichiometric proportion has no particularly adverse influences against proceeding of the reaction. The reaction temperature is usually in the range from room temperature to 300° C. or, preferably, from 50 to 150° C. When the reaction temperature is too low, the reaction does not proceed at a reasonable rate while, when the reaction temperature is too high, the catalytic platinum compound suffers thermal decomposition to decrease the catalytic activity.
The reactions according to the first and second methods of the invention are sensitive to the inhibiting effect of oxygen so that the reaction is performed preferably under an atmosphere of an inert gas such as nitrogen, argon and methane. The desired reaction product, which is a halogenosilyl thioalkene or bis(halogenosilyl thioalkene) expressed by the general formula (Ia) or (Ib), can easily be isolated from the reaction mixture by undertaking a known separating method such as chromatography, distillation and recrystallization.
The third method of the present invention employs the thus obtained halogenosilyl thioalkene or bis(halogenosilyl thioalkene) as one of the starting reagents in the preparation of a silyl thioalkene compound of the general formula (I) in which X is an unsubstituted or substituted monovalent hydrocarbon group. Namely, the above mentioned starting reagent is reacted with a hydrocarbon carbonium ion-generating agent so that the halogen atoms in the starting reagent are replaced with unsubstituted or substituted monovalent hydrocarbon groups. The carbonium ion-generating agent suitable in this case is exemplified by organic lithium compound such as methyl lithium, ethyl lithium, butyl lithium and phenyl lithium and so-called Grignard reagents such as methyl magnesium halides, ethyl magnesium halides, butyl magnesium halides and phenyl magnesium halides. The reaction of the halogenosilyl thioalkene compound with these carbonium ion-generating agent is performed in a reaction mixture of these reagents as diluted, usually, with an ether solvent at a temperature in the range from -20 to +20° C.
The fourth method of the present invention, which is for the preparation of a silyl thioalkene compound of the general formula (I) in which X is a hydrocarbyloxy group, utilizes also the halogenosilyl thioalkene compound obtained by the first or second method as one of the starting reagents. Namely, the halogenosilyl thioalkene compound is reacted with an alcohol compound in the presence of a dehydrohalogenating agent so that the halogen atoms in the starting reagent are replaced with hydrocarbyloxy groups. Examples of the alcohol compounds usable here include methyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, phenol and benzyl alcohol. The dehydrohalogenating agent suitable in this case is exemplified by organic basic compounds such as trimethyl amine, triethyl amine and pyridine. The dehydrohalogenation reaction is performed in a reaction mixture diluted with an organic solvent such as hydrocarbon solvents and ether solvents at a temperature in the range from -20 to +20° C.
The desired reaction products produced by the third and fourth methods of the invention can readily be isolated from the respective reaction mixtures by a conventional separating method such as chromatography, distillation and recrystallization.
Thus, the silyl thioalkene compound and the bis(silyl thioalkene) compound represented by the general formulas (Ia) and (Ib), respectively, can be obtained by undertaking the above described first to fourth methods according to the invention.
Identification of the inventive compound can be performed according to a conventional procedure by means of elementary analysis, 1 H-NMR and 13 C-NMR spectrometric measurements, infrared absorption spectrophotometry, mass spectrometry and others.
In the following, the method of the invention for the preparation of the novel compounds and characterization thereof are described in more detail by way of Examples, which, however, never limit the scope of the invention in any way.
EXAMPLE 1
A reaction mixture was prepared by the addition of, into 1 ml of toluene, 1 mmole of trichlorosilyl phenyl sulfide and 1 mmole of 1-octyne together with ethylenebis (triphenylphosphine)platinum as a catalyst in an amount of 5% by moles based on the amount of sulfur and the reaction mixture was heated at 110° C. for 24 hours under an atmosphere of nitrogen to effect the reaction. The reaction mixture was concentrated by removing toluene followed by distillation under reduced pressure to give a reaction product, which could be identified from the analytical results shown below to be (Z)-2-(phenylthio)-1-(trichlorosilyl)-1-octene which was a novel compound not described in any literatures. The yield of this product was 67% of the theoretical value.
1 H-NMR (C 6 D 6 ), δ, ppm: 7.21-7.24 (m, 2H); 6.87-6.94 (m, 3H); 5.78 (s, 1H); 1.96 (t, 2H, J=7.4 Hz); 0.95-1.24 (m, 8H); 0.79 (t, 3H, J=7.2 Hz)
13 C-NMR (C 6 D 6 ), δ, ppm: 166.6; 133.0; 129.4; 128.5; 127.2; 123.4; 38.9; 31.6; 28.5; 28.4; 22.7; 14.2
Infrared absorption spectrum (liquid film), cm -1 : 2960; 2936; 2862; 1562; 1479; 1439; 1069; 1025; 743; 690
Elementary analysis: calculated, %, as C 14 H 19 Cl 3 SSi: C 47.53; H 5.41; found, %: C 47.41; H 5.47
HRMS (EI, 70 eV): calculated: 352.0041; found: 352.0062
EXAMPLE 2
A reaction mixture was prepared by the addition of, into 3 ml of toluene, 1.5 mmoles of hexachlorodisilane, 1.5 mmoles of diphenyl disulfide and 3 mmoles of 1-octyne together with ethylenebis(triphenylphosphine)platinum as a catalyst in an amount of 1.5% by moles based on the amount of sulfur and the reaction mixture was heated at 110° C. for 12 hours under an atmosphere of nitrogen to effect the reaction. The reaction mixture was concentrated by removing toluene followed by distillation under reduced pressure to give a reaction product, which could be identified from the analytical results, which were substantially identical with those in Example 1, to be (Z)-2-(phenylthio)-1-(trichlorosilyl)-1-octene. The yield of this product was 63% of the theoretical value.
EXAMPLE 3
A reaction mixture was prepared by the addition of, into 3 ml of toluene, 1.5 mmoles of hexachlorodisilane, 1.5 mmoles of diphenyl disulfide and 3 mmoles of 1-octyne together with ethylenebis(triphenylphosphine)platinum as a catalyst in an amount of 1.5% by moles based on the amount of sulfur and the reaction mixture was heated at 110° C. for 12 hours under an atmosphere of nitrogen to effect the reaction. The reaction product isolated from the reaction mixture could be identified to be (Z)-2-(phenylthio)-1-(trichlorosilyl)-1-octene from the results of the NMR analysis. The yield of this product was 73% of the theoretical value.
EXAMPLE 4
The reaction mixture after completion of the reaction in Example 3 containing (Z)-2-(phenylthio)-1-(trichlorosilyl)-1-octene was admixed with 30 ml of diethyl ether and the reaction thereof was effected with 9 mmoles of methyl lithium as a 1 mole/liter ether solution at 0° C. for 0.5 hour. With admixture of 10 ml of water, the reaction mixture was extracted with ether and the extract solution was freed from the solvent by distillation under reduced pressure. The residue was subjected to distillation to give a product which could be identified to be (Z)-2-(phenylthio)-1-(trimethylsilyl)-1-octene from the NMR spectrometric analytical data given below. This compound is a novel compound not described in any literatures. The yield of the product was 65% of the theoretical value.
1 H-NMR (C 6 D 6 ), δ, ppm: 7.32-7.35 (m, 2H); 6.92-7.03 (m, 3H); 6.03 (s, 1H); 2.26 (t, 2H, J=7.1 Hz); 1.11-1.55 (m, 8H); 0.81 (t, 3H, J=6.9 Hz); 0.34 (s, 9H)
13 C-NMR (C 6 D 6 ), δ, ppm: 153.5; 135.9; 135.4; 130.8; 129.2; 126.7; 40.2; 32.0; 28.9; 28.8; 22.9; 14.2; 0.12
29 Si-NMR (C 6 D 6 ), δ, ppm: -9.9
HRMS (EI, 70 eV): calculated as C 17 H 28 SSi: 292.1661; found: 292.1659
EXAMPLE 5
A reaction mixture was prepared by the addition of, into 3 ml of toluene, 1.5 mmoles of hexachlorodisilane, 1.5 mmoles of bis(4-chlorophenyl) disulfide and 3 mmoles of 1-octyne together with ethylenebis(triphenylphosphine)platinum as a catalyst in an amount of 1.5% by moles based on the amount of sulfur and the reaction mixture was heated at 110° C. for 12 hours under an atmosphere of nitrogen to effect the reaction. The reaction product isolated from the reaction mixture could be identified to be (Z)-2-(4-chlorophenylthio)-1-(trichlorosilyl)-1-octene from the results of the NMR analysis. The yield of this product was 93% of the theoretical value.
EXAMPLE 6
The reaction mixture after completion of the reaction in Example 5 containing (Z)-2-(4-chlorophenylthio)-1-(trichlorosilyl)-1-octene was admixed with 30 ml of diethyl ether and further admixed at 0° C. with 10 mmoles of triethylamine and 10 mmoles of ethyl alcohol to effect the reaction for 0.5 hour. After removal of the precipitates by filtration, the filtrate was concentrated by distillation and the thus concentrated liquid was subjected to liquid chromatography to obtain an isolated reaction product which could be identified to be (Z)-2-(4-chlorophenylthio)-1-(triethoxysilyl)-1-octene from the spectrometric analytical data given below. This compound was a novel compound not described in any literatures. The yield of the product was 83% of the theoretical value.
1 H-NMR (C 6 D 6 ), δ, ppm: 7.11-7.15 (m, 2H); 6.92-6.97 (m, 2H); 5.94 (s, 1H); 3.97 (q, 6H, J=7.0 Hz); 2.13 (t, 2H, J=7.4 Hz); 1.27-1.43 (m, 2H); 1.25 (t, 9H, J=7.0 Hz); 1.05-1.21 (m, 6H); 0.81 (t, 3H, J=6.8 Hz)
13 C-NMR (C 6 D 6 ), δ, ppm: 157.0; 133.6; 133.4; 133.0; 129.3; 126.3; 58.8; 39.6; 31.8; 28.8; 28.6; 22.8; 18.6; 14.2
29 Si-NMR (C 6 D 6 ), δ, ppm: -61.1
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2930; 1580; 1477; 1390; 1168; 1083; 961; 820; 774
Elementary analysis: calculated, %, as C 20 H 33 ClO 3 SSi: C 57.60; H 7.97; found, %: C 57.61; H 7.80
HRMS (EI, 70 eV): calculated: 416.1606; found: 416.1496
EXAMPLE 7
Benzylacetylene as a starting reactant was reacted with hexachlorodisilane and bis(4-chlorophenyl) disulfide in the same manner as in Example 5 followed by a further reaction with ethyl alcohol in the same manner as in Example 6 to give (Z)-2-(4-chlorophenylthio)-3-phenyl-1-(triethoxysilyl)-1-propene, which was a novel compound not described in any literatures, in a yield of 76% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.20-7.33 (m, 7H); 6.99-6.02 (m, 2H); 5.65 (s, 1H); 3.90 (q, 6H, J=7.0 Hz); 3.45 (s, 2H); 1.24 (t, 9H, J=7.0 Hz)
13 C-NMR (CDCl 3 ), δ, ppm: 156.2; 137.9; 133.7; 133.6; 132.4; 129.1; 129.0; 128.4; 126.6; 125.7; 58.7; 45.6; 18.3
29 Si-NMR (CDCl 3 ), δ, ppm: -60.8
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2926; 2888; 1582; 1477; 1390; 1168; 1083; 1013; 961; 822; 754; 698
Elementary analysis: calculated, %, as C 21 H 27 ClO 3 SSi: C 59.62; H 6.43; found, %: C 59.55; H 6.42
HRMS (EI, 70 eV): calculated: 422.1137; found: 422.1154
EXAMPLE 8
(Z)-1-(4-Chlorophenylthio)-1-phenyl-2-(triethoxysilyl)ethene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with phenyl-acetylene. The yield of this product was 62% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (C 6 D 6 ), δ, ppm: 7.46-7.49 (m, 2H); 6.73-7.02 (m, 7H); 6.41 (s, 1H); 3.98 (q, 6H, J=7.0 Hz); 1.26 (t, 9H, J=7.0 Hz)
13 C-NMR (C 6 D 6 ), δ, ppm: 154.2; 140.4; 134.3; 132.5; 131.3; 130.7; 129.3; 128.9; 128.5; 128.1; 59.0; 18.6
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2888; 1555; 1477; 1446; 1390; 1168; 1081; 963; 777
HRMS (EI, 70 eV): calculated as C 20 H 25 ClO 3 SSi: 408.0981; found: 408.1064
EXAMPLE 9
(Z)-1-(4-Chlorophenyl)-1-(4-chlorophenylthio)-2-(triethoxysilyl)ethene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 4-chlorophenylacetylene. The yield of this product was 65% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.45-7.48 (m, 2H); 7.15-7.18 (m, 2H); 7.07-7.08 (m, 4H); 6.17 (s, 1H); 3.92 (q, 6H, J=7.1 Hz); 1.25 (t, 9H, J=7.1 Hz)
13 C-NMR (CDCl 3 ), δ, ppm: 153.1; 138.5; 134.7; 133.3; 132.5; 131.1; 129.1; 128.9; 128.8; 128.3; 58.9; 18.3
29 Si-NMR (CDCl 3 ), δ, ppm: -61.9
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2928; 2890; 1593; 1574; 1555; 1477; 1392; 1168; 1094; 1013; 963; 816; 775
Elementary analysis: calculated, %, as C 20 H 24 Cl 2 O 3 SSi: C 54.17; H 5.45; S 7.23; found, %: C 54.47; H 5.39; S 7.51
HRMS (EI, 70 eV): in calculated: 442.0591; found: 442.0492
EXAMPLE 10
(Z)-1-(4-Chlorophenylthio)-1-(4-methylphenyl)-2-(triethoxysilyl)ethene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 4-methylphenylacetylene. The yield of this product was 60% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (C 6 D 6 ), δ, ppm: 7.44-7.46 (m, 2H); 6.97-7.01 (m, 2H); 6.75-6.79 (m, 4H); 6.46 (s, 1H); 4.00 (q, 6H, J=7.0 Hz); 1.89 (s, 3H); 1.22 (t, 9H, J=7.0 Hz)
13 C-NMR (C 6 D 6 ), δ, ppm: 154.0; 138.9; 137.5; 134.6; 132.4; 131.2; 129.2; 129.1; 128.9; 128.1; 59.0; 20.9; 18.6
29 Si-NMR (C 6 D 6 ), δ, ppm: -61.4
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2926; 2888; 1557; 1506; 1477; 1390; 1168; 1083; 963; 903; 812; 772
Elementary analysis: calculated, %, as C 21 H 27 ClO 3 SSi: C 59.62; H 6.43; found, %: C 59.85; H 6.32
HRMS (EI, 70 eV): calculated: 422.1136; found: 422.1135
EXAMPLE 11
(Z)-5-Chloro-2-(4-chlorophenylthio)-1-(triethoxysilyl)-1-pentene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 5-chloro-1-pentyne. The yield of this product was 79% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.25-7.32 (m, 4H); 5.74 (s, 1H); 3.88 (q, 6H, J=7.1 Hz); 3.42 (t, 2H, J=6.5 Hz); 2.34 (t, 2H, J=7.2 Hz); 1.87-1.93 (m, 2H); 1.23 (t, 9H, J=7.1 Hz)
13 C-NMR (CDCl 3 ), δ, ppm: 155.5; 133.6; 133.1; 132.3; 129.2; 125.6; 58.7; 43.8; 36.2; 30.9; 18.3
29 Si-NMR (CDC 3 ), δ, ppm: -61.4
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2928; 2890; 1580; 1477; 1444; 1390; 1294; 1168; 1083; 1013; 963; 820; 764
Elementary analysis: calculated, %, as C 17 H 26 Cl 2 O 3 SSi: C 49.87; H 6.40; found, %: C 49.52; H 6.10
HRMS (EI, 70 eV): calculated: 408.0747; found: 408.0746
EXAMPLE 12
(Z)-5-Cyano-2-(4-chlorophenylthio)-1-(triethoxysilyl)-1-pentene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 5-cyano-1-pentyne. The yield of this product was 81% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (C 6 D 6 ), δ, ppm: 6.93-7.03 (m, 4H); 5.76 (s, 1H); 3.92 (q, 6H, J=7.0 Hz); 1.91 (t, 2H, J=7.3 Hz); 1.36 (t, 2H, J=6.8 Hz); 1.15-1.25 (m, 2H); 1.21 (t, 9H, J=7.0 Hz)
13 C-NMR (C 6 D 6 ), δ, ppm: 154.2; 133.8; 133.0; 132.7; 129.5; 128.1; 118.8; 58.9; 37.8; 24.0; 18.6; 15.5
29 Si-NMR (C 6 D 6 ), δ, ppm: -61.9
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2928; 2890; 2250; 1580; 1477; 1441; 1390; 1168; 1081; 1013; 963; 820; 777
Elementary analysis: calculated, %, as Cl 18 H 26 ClNO 3 SSi: C 54.05; H 6.55; N 3.50; found, %: C 53.87; H 6.59; N 3.59
HRMS (EI, 70 eV): calculated: 399.1090; found: 399.1097
EXAMPLE 13
(Z)-6-(tert-Butyldimethylsiloxy)-2-(4-chlorophenylthio)-1-(triethoxysilyl)-1-hexene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 6-(tert-butyldimethylsiloxy)-1-hexyne. The yield of this product was 72% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.23-7.32 (m, 4H); 5.68 (s, 1H); 3.86 (q, 6H, J=7.0 Hz); 3.51 (t, 2H, J=6.4 Hz); 2.18 (t, 2H, J=7.4 Hz); 1.21-1.25 (m, 4H); 1.23 (t, 9H, J=7.0 Hz); 0.86 (s, 9H); 0.00 (s, 6H)
13 C-NMR (CDCl 3 ), δ, ppm: 157.5; 133.4; 133.1; 132.8; 129.1; 123.9; 62.8; 58.6; 38.9; 31.9; 25.9; 24.7; 18.3; 18.2; -5.3
29 Si-NMR (CDCl 3 ), δ, ppm: 18.5; -60.7
Infrared absorption spectrum (liquid film), cm -1 : 2932; 2139; 1257; 1168; 1083; 1013; 961; 835; 777
Elementary analysis: calculated, %, as C 24 H 43 ClO 4 SSi 2 : C 55.51; H 8.35; S 6.17; found, %: C 55.58; H 8.41; S 6.40
EXAMPLE 14
(Z)-4-(tert-Butylcarbonyloxy)-2-(4-chlorophenylthio)-1-(triethoxysilyl)-1-butene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with 4-(tert-butylcarbonyloxy)-1-butyne. The yield of this product was 87% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.24-7.32 (m, 4H); 5.78 (s, 1H); 4.12 (t, 2H, J=6.3 Hz); 3.86 (q, 6H, J=7.1 Hz); 2.49 (t, 2H, J=6.3 Hz); 1.21 (t, 9H, J=7.1 Hz); 1.14 (s, 9H)
13 C-NMR (CDCl 3 ), δ, ppm: 178.3; 152.5; 133.5; 132.8; 132.4; 129.3; 127.8; 61.9; 58.6; 38.7; 38.2; 27.1; 18.2
29 Si-NMR (CDCl 3 ), δ, ppm: -61.8
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2930; 1731; 1584; 1477; 1392; 1286; 1156; 1087; 963; 822; 772
Elementary analysis: calculated, %, as C 21 H 33 ClO 5 SSi: C 54.70; H 7.21; found, %: C 54.54; H 7.27
HRMS (EI, 70 eV): calculated: 460.1504; found : 460.1449
EXAMPLE 15
(Z,Z)-1,3-Bis(triethoxysilyl)-2,7-bis(4-chlorophenylthio)-nona-1,8-diene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with n-nona-1,8-diyne and increase of the amounts of hexachlorodisilane and bis(4-chlorophenyl) disulfide each from 1.5 mmoles to 3.0 mmoles. The yield of this product was 69% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (CDCl 3 ), δ, ppm: 7.23-7.29 (m, 8H); 5.63 (s, 2H); 3.87 (q, 12H, J=6.9 Hz); 2.09 (t, 4H, J=7.5 Hz); 1.34-1.39 (m, 4H); 1.23 (t, 18H, J=6.9 Hz); 1.02-1.05 (m, 2H)
13 C-NMR (CDCl 3 ), δ, ppm: 157.4; 133.4; 133.0; 132.7; 129.1; 123.9; 58.6; 39.0; 28.1; 27.9; 18.3
29 Si-NMR (CDCl 3 ), δ, ppm: -60.8
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2930; 1580; 1477; 1441; 1390; 1294; 1168; 1077; 1013; 961; 820; 777; 745
Elementary analysis: calculated, %, as C 33 H 50 Cl 2 O 6 S 2 Si 2 : C 54.00; H 6.87; found, %: C 54.32; H 6.70
EXAMPLE 16
(Z)-1-(4-Chlorophenylthio)-1-(1-cyclohexenyl)-2-(triethoxysilyl)ethene was prepared in the same manner as in Example 7 excepting for replacement of benzylacetylene with cyclohexen-1-ylacetylene. The yield of this product was 51% of the theoretical value.
The results obtained in the analysis of this product were as follows.
1 H-NMR (C 6 D 6 ), δ, ppm: 6.92-7.05 (m, 4H); 6.36 (bs, 1H); 6.24 (s, 1H); 3.90 (q, 6H, J=7.0 Hz); 1.98-2.00 (m, 2H); 1.74-1.76 (m, 2H); 1.20 (t, 9H, J=7.0 Hz); 1.11-1.31 (m, 4H)
13 C-NMR (C 6 D 6 ), δ, ppm: 154.4; 136.3; 136.2; 132.0; 131.8; 130.1; 128.9; 127.2; 58.9; 27.3; 26.0; 22.9; 21.9; 18.5
29 Si-NMR (C 6 D 6 ), δ, ppm: -60.9
Infrared absorption spectrum (liquid film), cm -1 : 2976; 2928; 1549; 1477; 1390; 1168; 1093; 963; 774; 714
Elementary analysis: calculated, %, as C 20 H 29 ClO 3 SSi: C 58.16; H 7.08; found, %: C 58.34; H 7.05
HRMS (EI, 70 eV): calculated: 412.1294; found: 412.1395 | Disclosed is a silyl thioalkene compound, as a class of organosilicon compounds, represented by the general formula
R(--CSAr═CHSiX.sub.3).sub.n,
in which the subscript n is 1 or 2, R is, when n is 1, a hydrogen atom or unsubstituted or substituted monovalent hydrocarbon group or, when n is 2, a divalent hydrocarbon group, Ar is an unsubstituted or nucleus-substituted aromatic monovalent aromatic hydrocarbon group and X is a halogen atom, a monovalent hydrocarbon group or hydrocarbyloxy group, having usefulness as an intermediate in the synthesis of various precision organic chemicals. The compound, of which X is a halogen atom X 1 , can be prepared, for example, by the reaction of an alkyne compound of the general formula
R(--C.tbd.CH).sub.n,
with a silyl sulfide compound of the general formula
ArS--SiX.sup.1.sub.3,
in the presence of a platinum complex catalyst. The compound, of which X is a monovalent hydrocarbon group or a hydrocarbyloxy group, can be derived from the above obtained halogen-containing compound. | 2 |
COPYRIGHT & TRADEMARK NOTICES
[0001] A portion of the disclosure of this patent document contains material, which is subject to copyright protection. The owner has no objection to the facsimile reproduction by any one of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent file or records, but otherwise reserves all copyrights whatsoever.
[0002] Certain marks referenced herein may be common law or registered trademarks of third parties affiliated or unaffiliated with the applicant or the assignee. Use of these marks is for providing an enabling disclosure by way of example and shall not be construed to limit the scope of the claimed subject matter to material associated with such marks.
TECHNICAL FIELD
[0003] The claimed subject matter relates generally to nested virtualization and, more particularly, to para-virtualization in a nested virtualization environment.
[0004] In a virtualization environment, a host software running on one or more hardware infrastructures may emulate the hardware for a guest software running on the host software. In other words, a hypervisor running on a physical machine may implement a virtual machine (VM) for a guest running on the hypervisor. That is, the VM may allow the guest to operate as if the guest were running directly on the physical machine.
[0005] Typically, the physical machine operates in a guest mode or a root mode. In the guest mode, the guest software manages execution of instructions by the physical machine. In the root mode, the hypervisor manages execution of instructions by the physical machine. The physical machine generally operates in the guest mode, but may switch to the root mode to execute a privileged instruction that requires support from the hypervisor to be compatible with the physical machine. Switching to the root mode is referred to as a VM exit, and switching back to the guest mode is referred to as a VM entry.
SUMMARY
[0006] The present disclosure is directed to systems and corresponding methods that facilitate para-virtualization in a nested virtualization environment.
[0007] For purposes of summarizing, certain aspects, advantages, and novel features have been described herein. It is to be understood that not all such advantages may be achieved in accordance with any one particular embodiment. Thus, the claimed subject matter may be embodied or carried out in a manner that achieves or optimizes one advantage or group of advantages without achieving all advantages as may be taught or suggested herein.
[0008] In accordance with one embodiment, a para-virtualization method is provided. The method comprises implementing a virtual machine (VM) for guest software running on first host software. In response to a privileged instruction, the guest software causes a first VM exit. If the first host software is not running directly on hardware, the privileged instruction is managed without causing a second VM exit. Otherwise, the privileged instruction is managed normally.
[0009] In accordance with another embodiment, a system comprising one or more logic units is provided. The one or more logic units are configured to perform the functions and operations associated with the above-disclosed methods. In accordance with yet another embodiment, a computer program product comprising a computer useable medium having a computer readable program is provided. The computer readable program when executed on a computer causes the computer to perform the functions and operations associated with the above-disclosed methods.
[0010] One or more of the above-disclosed embodiments in addition to certain alternatives are provided in further detail below with reference to the attached figures. The claimed subject matter is not, however, limited to any particular embodiment disclosed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Embodiments of the claimed subject matter are understood by referring to the figures in the attached drawings, as provided below.
[0012] FIG. 1 illustrates an exemplary nested virtualization environment, in accordance with one or more embodiments.
[0013] FIG. 2 is a flow diagram of a method for managing a privileged instruction, in accordance with one embodiment.
[0014] FIG. 3 is a flow diagram of a first method for determining whether a hypervisor is a nested hypervisor.
[0015] FIG. 4 is a flow diagram of a second method for determining whether a hypervisor is a nested hypervisor.
[0016] FIG. 5 illustrates an exemplary nested virtualization environment, in accordance with one embodiment.
[0017] FIG. 6 is a flow diagram of a method for initializing a nested para-virtualization environment, in accordance with one embodiment.
[0018] FIG. 7 is a flow diagram of a method for managing a privileged instruction, in accordance with one embodiment.
[0019] FIGS. 8 and 9 are block diagrams of hardware and software environments in which a system of the present invention may operate, in accordance with one or more embodiments.
[0020] Features, elements, and aspects that are referenced by the same numerals in different figures represent the same, equivalent, or similar features, elements, or aspects, in accordance with one or more embodiments.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0021] In the following, numerous specific details are set forth to provide a thorough description of various embodiments of the claimed subject matter. Certain embodiments may be practiced without these specific details or with some variations in detail. In some instances, certain features are described in less detail so as not to obscure other aspects of the disclosed embodiments. The level of detail associated with each of the elements or features should not be construed to qualify the novelty or importance of one feature over the others.
[0022] Para-virtualization refers to the ability of a guest software to communicate with a root hypervisor using one or more hypercalls provided in an application programming interface (API). As a result, some of the functionality provided by the root hypervisor may be provided by the guest instead.
[0023] In one or more embodiments, para-virtualization may be implemented for a nested hypervisor (i.e., a hypervisor running as a guest on another hypervisor) and a root hypervisor. In one implementation, if a guest running on the nested hypervisor causes a VM exit due to a privileged instruction, the nested hypervisor may manage the privileged instruction without causing another VM exit. Depending on the level of nesting, such an implementation may reduce the number of VM exits several orders of magnitude. Since each VM exit is associated with an overheard cost, the reduction of VM exits may significantly improve performance.
[0024] Referring to FIG. 1 , in accordance with one or more embodiments, para-virtualization may be implemented in an exemplary nested virtualization environment 100 comprising a physical machine 110 and a level 0 (L0), or root, hypervisor 120 , and one or more higher-level, or nested, hypervisors. The level 1 (L0) hypervisor 120 runs on the physical machine 110 , and one or more guests run on the L0 hypervisor 120 and each of the higher-level hypervisors. For example, the guest 150 runs as a guest on the level 2 (L2) hypervisor 140 ; the L2 hypervisor 140 runs as a guest on the level 1 (L1) hypervisor 130 ; and the L1 hypervisor 130 runs as a guest on the L0 hypervisor 120 .
[0025] Referring to FIGS. 1 and 2 , in accordance with one or more embodiments, a guest running on a hypervisor causes a VM exit to the root hypervisor (e.g., the L0 hypervisor 120 ) due to a privileged instruction (P 200 ).
[0026] If the guest is running on a para-virtualized nested hypervisor (e.g., the L1 hypervisor 130 or the L2 hypervisor 140 ) (P 210 ), the root hypervisor traps to the next-level hypervisor (e.g., the L1 hypervisor 130 ) (P 220 ). In other words, the root hypervisor throws an exception and transfers control to the next-level hypervisor to handle the exception. The next-level hypervisor manages the privileged instruction without causing another VM exit (P 230 ). If the guest is running on the root hypervisor, the root hypervisor manages the privileged instruction normally (P 240 ). It is noteworthy that the root hypervisor may mark para-virtualized nested hypervisors on startup, as provided in more detail below.
[0027] Referring to FIGS. 2 and 3 , in accordance with one embodiment, on startup or at some other point in time, a hypervisor performs a hypercall to determine whether the hypervisor is a nested hypervisor running on another hypervisor or the root hypervisor running directly on the hardware (P 300 ). The hypercall may be described in an API. If the hypercall fails (P 310 ), the hypervisor is determined to be the root hypervisor (P 320 ). Otherwise, the hypervisor is determined to be a nested hypervisor (P 330 ) and the hypervisor is marked as a para-virtualized nested hypervisor by the root hypervisor (P 340 ).
[0028] Referring to FIGS. 2 and 4 , in accordance with one embodiment, on startup or at some other point in time, the hypervisor requests an identification (ID) of the underlying hardware (e.g., performs a CPU_ID command) to determine whether the hypervisor is a nested hypervisor running on another hypervisor or the root hypervisor running directly on hardware (P 400 ). If the value of returned by the ID request is a value associated with a VM (P 410 ), the hypervisor is determined to be a nested hypervisor (P 420 ). Otherwise, the hypervisor is determined to be the root hypervisor (P 430 ).
[0029] A para-virtualization implementation is provided below for enabling a nested hypervisor to manage privileged instructions in an Intel VT-x virtualization environment. It should be understood, however, that such an implementation is provided for purposes of example to illustrate the processes described above. In other implementations, para-virtualization may be implemented for different types of privileged instructions in different types of virtualization environments, without limitation.
[0030] Referring to FIG. 5 , in accordance with one or more embodiments, an exemplary virtualization environment 500 (e.g., Intel VT-x) comprises a CPU 510 , a root hypervisor 520 , a nested hypervisor 530 , a guest 540 , and a memory 550 . The guest 540 is a guest that runs on the nested hypervisor 530 , and the nested hypervisor 530 is a guest that runs on the root hypervisor 520 .
[0031] Referring to FIGS. 5 and 6 , in accordance with one embodiment, the root hypervisor 520 implements a VM for the nested hypervisor 530 by creating a VM control structure (VMCS) 561 and loading the VMCS 561 into the memory 550 . The root hypervisor 520 also runs the nested hypervisor 530 (P 600 ). On startup, the nested hypervisor 530 performs a hypercall and determines that the nested hypervisor 530 is running on another hypervisor. In response to the hypercall, the root hypervisor 520 marks the nested hypervisor 530 as a para-virtualized nested hypervisor (P 610 ).
[0032] The nested hypervisor 530 implements a VM for the guest 540 by creating a VMCS 562 and calling a VMTPRLD instruction to load the VMCS 562 into the memory 550 . The VMTPRLD instruction causes a trap to the root hypervisor 520 , and the root hypervisor 520 saves the address of the VMCS 562 (P 620 ). In other words, the nested hypervisor 530 throws an exception and transfers control to the root hypervisor 520 to handle the exception.
[0033] Once the VMCS 562 is loaded into the memory 550 , the nested hypervisor 530 calls a VMLAUNCH instruction to run the guest 540 . The VMLAUNCH instruction causes a trap to the root hypervisor 520 , and the root hypervisor 520 creates a VMCS 563 and calls a VMTPRLD instruction to load the VMCS 563 into the memory 550 (P 630 ). The root hypervisor 520 also calls a VMLAUNCH instruction to run the guest 540 (P 640 ).
[0034] Referring to FIGS. 5 through 7 , in accordance with one embodiment, the guest 540 causes a VM exit due to a privileged instruction (e.g., VMREAD or VMWRITE) (P 700 ). In response to the VM exit, the root hypervisor 520 updates the VMCS 563 in the memory 550 with values from the VMCS 562 and runs the nested hypervisor (P 710 )
[0035] The nested hypervisor 530 reads from or writes to the VMCS 563 in the memory 550 (e.g., depending on whether the privileged instruction is a VMREAD or a VMWRITE instruction, respectively). In other words, the nested hypervisor 530 directly accesses the VMCS 563 (e.g., instead of calling the VMREAD or VMWRITE instruction again) to access the VMCS 562 and causing another VM exit. Once the memory access is completed, the nested hypervisor 530 calls a VMRESUME instruction to perform a VM entry (i.e., run the guest 540 again) (P 730 ).
[0036] The VMRESUME instruction causes a trap to the root hypervisor 520 , and the root hypervisor 520 updates the VMCS 563 with values from the VMCS 561 and the VMCS 562 . The root hypervisor 520 also calls a VMPTRLD instruction to load the VMCS 563 into the memory 550 (P 730 ) and calls a VMLAUNCH instruction to run the guest 540 (P 740 ).
[0037] Alternatively, instead of directly accessing the VMCS 563 in the memory 550 , the nested hypervisor 530 may perform a hypercall that batches several privileged instructions (e.g., VMREADs and VMWRITEs) to reduce the number of VM exits.
[0038] In different embodiments, the claimed subject matter may be implemented either entirely in the form of hardware or entirely in the form of software, or a combination of both hardware and software elements. For example, a nested virtualization environment may comprise a controlled computing system environment that may be presented largely in terms of hardware components and software code executed to perform processes that achieve the results contemplated by the system of the claimed subject matter.
[0039] Referring to FIGS. 8 and 9 , a computing system environment in accordance with an exemplary embodiment is composed of a hardware environment 1110 and a software environment 1120 . The hardware environment 1110 comprises the machinery and equipment that provide an execution environment for the software; and the software environment 1120 provides the execution instructions for the hardware as provided below.
[0040] As provided here, software elements that are executed on the illustrated hardware elements are described in terms of specific logical/functional relationships. It should be noted, however, that the respective methods implemented in software may be also implemented in hardware by way of configured and programmed processors, ASICs (application specific integrated circuits), FPGAs (Field Programmable Gate Arrays) and DSPs (digital signal processors), for example.
[0041] Software environment 1120 is divided into two major classes comprising system software 1121 and application software 1122 . In one embodiment, a hypervisor may be implemented as system software 1121 or application software 1122 executed on one or more software or hardware environments to facilitate para-virtualization in a nested virtualization environment.
[0042] System software 1121 may comprise control programs, such as the operating system (OS) and information management systems that instruct the hardware how to function and process information. Application software 1122 may comprise but is not limited to program code, data structures, firmware, resident software, microcode or any other form of information or routine that may be read, analyzed or executed by a microcontroller.
[0043] In an alternative embodiment, the claimed subject matter may be implemented as computer program product accessible from a computer-usable or computer-readable medium providing program code for use by or in connection with a computer or any instruction execution system. For the purposes of this description, a computer-usable or computer-readable medium may be any apparatus that can contain, store, communicate, propagate or transport the program for use by or in connection with the instruction execution system, apparatus or device.
[0044] The computer-readable medium may be an electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system (or apparatus or device) or a propagation medium. Examples of a computer-readable medium include a semiconductor or solid-state memory, magnetic tape, a removable computer diskette, a random access memory (RAM), a read-only memory (ROM), a rigid magnetic disk and an optical disk. Current examples of optical disks include compact disk read only memory (CD-ROM), compact disk read/write (CD-R/W) and digital video disk (DVD).
[0045] Referring to FIG. 8 , an embodiment of the application software 1122 may be implemented as computer software in the form of computer readable code executed on a data processing system such as hardware environment 1110 that comprises a processor 1101 coupled to one or more memory elements by way of a system bus 1100 . The memory elements, for example, may comprise local memory 1102 , storage media 1106 , and cache memory 1104 . Processor 1101 loads executable code from storage media 1106 to local memory 1102 . Cache memory 1104 provides temporary storage to reduce the number of times code is loaded from storage media 1106 for execution.
[0046] A user interface device 1105 (e.g., keyboard, pointing device, etc.) and a display screen 1107 can be coupled to the computing system either directly or through an intervening I/O controller 1103 , for example. A communication interface unit 1108 , such as a network adapter, may be also coupled to the computing system to enable the data processing system to communicate with other data processing systems or remote printers or storage devices through intervening private or public networks. Wired or wireless modems and Ethernet cards are a few of the exemplary types of network adapters.
[0047] In one or more embodiments, hardware environment 1110 may not include all the above components, or may comprise other components for additional functionality or utility. For example, hardware environment 1110 can be a laptop computer or other portable computing device embodied in an embedded system such as a set-top box, a personal data assistant (PDA), a mobile communication unit (e.g., a wireless phone), or other similar hardware platforms that have information processing and/or data storage and communication capabilities.
[0048] In some embodiments of the system, communication interface 1108 communicates with other systems by sending and receiving electrical, electromagnetic or optical signals that carry digital data streams representing various types of information including program code. The communication may be established by way of a remote network (e.g., the Internet), or alternatively by way of transmission over a carrier wave.
[0049] Referring to FIG. 9 , application software 1122 may comprise one or more computer programs that are executed on top of system software 1121 after being loaded from storage media 1106 into local memory 1102 . In a client-server architecture, application software 1122 may comprise client software and server software. For example, in one embodiment, client software is executed on a personal computing system (not shown) and server software is executed on a server system (not shown).
[0050] Software environment 1120 may also comprise browser software 1126 for accessing data available over local or remote computing networks. Further, software environment 1120 may comprise a user interface 1124 (e.g., a Graphical User Interface (GUI)) for receiving user commands and data. Please note that the hardware and software architectures and environments described above are for purposes of example, and one or more embodiments of the invention may be implemented over any type of system architecture or processing environment.
[0051] It should also be understood that the logic code, programs, modules, processes, methods and the order in which the respective processes of each method are performed are purely exemplary. Depending on implementation, the processes can be performed in any order or in parallel, unless indicated otherwise in the present disclosure. Further, the logic code is not related, or limited to any particular programming language, and may comprise of one or more modules that execute on one or more processors in a distributed, non-distributed or multiprocessing environment.
[0052] The claimed subject matter has been described above with reference to one or more features or embodiments. Those skilled in the art will recognize, however, that changes and modifications may be made to these embodiments without departing from the scope of the claimed subject matter. These and various other adaptations and combinations of the embodiments disclosed are within the scope of the claimed subject matter as defined by the claims and their full scope of equivalents. | A para-virtualization method is provided. The method comprises implementing a virtual machine (VM) for guest software running on first host software. In response to a privileged instruction, the guest software causes a first VM exit. If the first host software is not running directly on hardware, the privileged instruction is managed without causing a second VM exit. Otherwise, the privileged instruction is managed normally. | 6 |
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. patent application Ser. No. 14/100,658, filed Dec. 9, 2013, now U.S. Pat. No. 9,183,425, which is a continuation of U.S. patent application Ser. No. 13/459,698, filed Apr. 30, 2012, now U.S. Pat. No. 8,603,437, which is a continuation of U.S. patent application Ser. No. 12/418,563, filed Apr. 3, 2009, now U.S. Pat. No. 8,168,159, which is a continuation of U.S. patent application Ser. No. 09/839,779, filed Apr. 20, 2001, now U.S. Pat. No. 7,514,067, which claims the benefit of priority to U.S. Provisional Patent Application No. 60/199,350, filed Apr. 25, 2000, the specification, claims, and drawings (if any) of all of which are hereby incorporated by reference into the specification of this application.
BACKGROUND OF THE INVENTION
[0002] Monoclonal antibodies (MAb), by virtue of their unique in-vitro specificity and high affinity for their antigen, have generally been considered particularly attractive as selective carriers of cancer radiodiagnostic/therapeutic agents. Several reasons underlie these expectations: (i) they show a high degree of specificity and affinity for their intended target; (ii) they are generally nontoxic; and (iii) they can transport such agents. The application of MAb in animals and humans for both tumor scintigraphic detection (labeled with 123 I, 131 I, 93m Tc, and 111 In) and therapy (labeled with the beta emitters 131 I, 186 Re, 90 Y, 165 Dy, 67 Cu, and 109 Pd; the alpha emitters 211 At, and 212 Bi, and 213 Bi; or conjugated to various toxins and cytotoxic drugs) is the focus of work in many research laboratories.
[0003] In pursuing these studies, the basic assumption continues to be that MAb have a role in the radioimmunodiagnosis and radioimmunotherapy of cancer. However, while most published work on this subject has demonstrated their utility in the diagnosis and treatment of various tumors in experimental animal models, the use of radiolabeled MAb to target and treat solid tumors in cancer patients has been for the most part unsuccessful. There are at least five reasons for the results seen in humans:
1. Low Tumor Uptake. Thus far, most studies in humans have demonstrated that the percentage injected dose per gram of tumor (% ID/g) is extremely low. As a result, the absolute amount of the therapeutic radionuclide within the tumor is much less than that needed to deposit a radiation dose sufficiently high to sterilize the tumor. 2. High Activity in the Whole Body. A corollary to low tumor uptake is the presence of ˜90%-99% of the injected radiolabeled MAb in the rest of the body. This has led to the deposition of high doses in normal tissues and unacceptable side effects, and a reduction in the maximum tolerated dose (MTD). 3. Slow Blood Clearance. In most human radioimmunotherapy trials, whole MAb (MW ˜150,000 Da) have been used. The clearance of such high-molecular-weight proteins from blood and nontargeted tissues is rather slow. The resulting systemic exposure to the radioisotope thus produces high doses to the bone marrow and a lowering of the MTD. 4. Limited Intratumoral Diffusion. The high molecular weight of MAb also limits their ability to extravasate and diffuse through the tumor mass. As a consequence, many areas within the tumor are spared from receiving a lethal dose of radiation (i.e., the areas are either outside the range of the emitted particle or receive a sublethal dose). 5. Heterogeneity of Tumor-Associated Antigen Expression. Many studies have demonstrated that a substantial proportion of the cells within a tumor mass show reduced/no expression of the targeted antigen. This also will lead to nonuniform distribution of the radionuclide within the tumor mass and the sparing of a large number of cells within the tumor.
[0009] In an attempt to bypass some of the limitations of these unique molecules, various two-step and three-step approaches have been theorized, in which a noninternalizing antitumor antibody is injected prior to the administration of a low-molecular-weight therapeutic molecule that has an affinity/reactivity with the preinjected antibody molecule. These systems can be categorized into two major classes: MAb-directed enzyme prodrug therapy and MAb-directed radioligand targeting, details of which are known in the art.
[0010] It is clear that under ideal conditions, a radiolabeled therapeutic agent must meet the following requirements: (i) be labeled with an energetic particle emitter, (ii) be taken up rapidly and efficiently by the tumor, (iii) be retained by the tumor (i.e. very long effective clearance half-life), (iv) have a short residence within normal tissues (i.e., short effective half-life in blood, bone marrow, and whole body), (v) achieve high tumor-to-normal tissue uptake ratios, (vi) attain an intratumoral distribution that is sufficiently uniform to match the range of the emitted particles (i.e. all tumor cells are within the range of the emitted particles), and (vii) achieve an intratumoral concentration that is sufficiently high to deposit a tumoricidal dose in every cell that is within the range of the emitted particle.
SUMMARY OF THE INVENTION
[0011] The present invention relates to a method for the enzyme-mediated, site-specific, in-vivo precipitation of a water soluble molecule in an animal. The enzyme is either unique to tumor cells (i.e. only produced by tumor cells), or is produced within the specific site (e.g., tumor) at concentrations that are higher than that in normal tissues. Alternatively, the enzyme is conjugated to a targeting moiety such as an antibody. For example, an antibody-enzyme conjugate is injected into tumor bearing animals and following tumor targeting and clearance from normal tissues and organs, the water soluble substrate is injected. Owing to the negatively charged prosthetic group (e.g. phosphate) present within its molecules, the substrate is highly hydrophilic, is not internalized by mammalian cells, and should clear from circulation at a rate that is compatible with its physical characteristics (e.g. molecular weight, charge). However, being a substrate for the enzyme (pre-targeted or otherwise), this water soluble molecule loses the prosthetic group and the resulting molecule precipitates out due to its highly water-insoluble nature. The precipitated molecule is thus “indefinitely trapped” within the targeted tissue. In one of its aspects (Enzymatic Radiolabel Insolubilization Therapy, ERIT), the substrate is radiolabeled with a gamma or a positron emitting radionuclide and as such, the location of the precipitate can be detected by external imaging means (SPECT/PET). On the other hand, when the radionuclide is an alpha or a beta particle emitter, the trapped precipitated radioactive molecule will maintain the radionuclide within the targeted tumor thereby enhancing its residence time and delivering a high radiation dose specifically to the tumor relative to the rest of the body. In yet another aspect (Enzymatic Boron Insolubilization Therapy, EBIT), the substrate is conjugated to one/more boron-containing molecule and upon precipitation within its intended target, the tumor is subjected to epithermal neutrons with the subsequent alpha particle emissions (Boron Capture Therapy).
[0012] In its simplest form, therefore, the present invention is based on the conversion of a chemical (e.g. quinazolinones, benzoxazoles, benzimidazoles, benzothiazoles, indoles, and derivatives thereof) from a freely water-soluble form to a highly water-insoluble form and hence in vivo precipitation at the specific site where an enzyme (e.g. acetylglucosaminidases, acetylneuraminidases, aldolases, amidotranferases, arabinopayranosidases, carboxykinases, cellulases, deaminases, decarboxylases, dehydratases, dehydrogenase, DNAses, endonucleases, epimerases, esterases, exonucleases, fucosidases, galactosidases, glucokinases, glucosidases, glutaminases, glutathionases, guanidinobenzodases, glucoronidases, hexokinases, iduronidases, kinases, lactases, manosidases, nitrophenylphosphatases, peptidases, peroxidases, phosphatases, phosphotransferases, proteases, reductases, RNAses, sulfatases, telomerases, transaminases, transcarbamylases, transferases, xylosidases, uricases, urokinasess) or any other species capable of carrying out such a conversion in high concentrations. Pretargeting of enzyme or its equivalent species may be achieved by making use of specific antibodies or any such specific receptor-binding ligand to the desired sites in vivo. Note that the ligand may also be a peptide or hormone, with the receptor specific to the peptide or hormone.
[0013] Alternatively, the enzyme may be produced within the tumor site by the tumor cells themselves or following gene therapy or similar means. The chemical to be injected in the second step contains any nuclide suitable for imaging and/or therapy (e.g. Boron-10, Carbon-11, Nitrogen 13, Oxygen-15, Fluorine-18, Phosphorous-32, Phosphorous-33, Technetium-99m, Indium-111, Yttrium-90, Iodine-123, Iodine-124, Iodine-131, Astatine-211, Bismuth-212, etc.).
BRIEF DESCRIPTION OF THE DRAWINGS
[0014] The accompanying drawings illustrate preferred embodiments of the invention as well as other information pertinent to the disclosure, in which:
[0015] FIG. 1 is a graph of a time-course conversion of 1 (or Compound A) to 2 (or Compound B) following incubation in alkaline phosphatase;
[0016] FIG. 2 is an illustration of the conversion of 125 I-1 ( 125 I-labeled Compound A) to 125 I-2 ( 125 I-labeled Compound B) following incubation with ALP.
[0017] FIG. 3 is a graph of radioactivity following i.v. injection of 125 I-1 into mice.
[0018] FIG. 4 is an illustration of the biodistribution of 125 I-1 in normal mice.
[0019] FIG. 5 is an illustration of the biodistribution of 125 I-2 in normal mice.
[0020] FIG. 6 is a graph of the accumulation of radioactivity within forelimbs of mice after subcutaneous (s.c.) injection of alkaline phosphatase followed by i.v. injection of 125 I-2.
[0021] FIG. 7 is a graph depicting the retention of radioactivity within a forelimb of mice injected s.c. with 125 I-1 or 125 I-2.
[0022] FIG. 8 is an illustration of the biodistribution (24 hours) of s.c.-injected 125 I-2 in normal mice.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0023] This invention describes a novel approach that serves to localize water-insoluble, radioactive molecules within the extracellular (interstitial) space of a tumor. In one embodiment of this invention, a noninternalizing monoclonal antibody (MAb) to a “tumor-specific” antigen is chemically conjugated to the enzyme alkaline phosphatase (ALP); the MAb-ALP conjugate is administered intravenously (i.v.) to tumor-bearing animals, and after MAb-ALP tumor localization and clearance from circulation (high tumor to normal tissue ratios), a water-soluble, radiolabeled prodrug (PD) that is a substrate for ALP is injected intravenously. The conjugate or prodrug may also be injected intra-arterially, subcutaneously, into the lymphatic circulation, intraperitoneally, intrathecally, intratumorally, intravesically, or is given orally.
[0024] The prodrug substrate is represented by the following formula:
[0000] R 1 -D-(O-BLOCK) wherein BLOCK is a blocking group that can be cleaved from the remainder of the substrate by action of an enzyme, resulting in a water-insoluble drug molecule represented by the following formula:
[0000] R 1 -D-O—H
wherein D contains a minimum of 2 linked aromatic rings, and R 1 is a radioactive atom, a molecule labeled with one or more radioactive atom(s), a boron atom, or a molecule labeled with one or more boron atoms.
[0027] The radiolabel is selected from the group consisting of a gamma emitting radionuclide suitable for gamma camera imaging, a positron emitting radionuclide suitable for positron emission tomography, and an alpha or a beta particle emitting radionuclide suitable for therapy. The alpha particle emitting radionuclide may be, e.g., astatine-211, bismuth-212, or bismuth-213. The beta particle emitting radionuclide emits beta particles whose energies are greater than about 1 keV. The beta particle emitting radionuclide may be, e.g., iodine-131, copper-67, samarium-153, gold-198, palladium-109, rhenium-186, rhenium-188, dysprosium-165, strontium-89, phosphorous-32, phosphorous-33, or yttrium-90. Note also that the boron atom is suitable for neutron activation.
[0028] The BLOCK is selected from the group consisting of:
a monovalent blocking group derivable by removal of one hydroxyl from a phosphoric acid group, a sulfuric acid group, or a biologically compatible salt thereof; a monovalent blocking group derivable by removal of a hydroxyl from an alcohol or an aliphatic carboxyl, an aromatic carboxyl, an amino acid carboxyl, or a peptide carboxyl; and a monovalent moiety derived by the removal of the anomeric hydroxyl group from a mono- or polysaccharide.
[0032] As the PD molecules percolate through the tumor mass, they will be hydrolyzed by the ALP molecules present within the tumor (MAb-ALP). The hydrolysis of PD (Compound 1, or Compound A below) leads to the formation of a water-insoluble, radiolabeled precipitate (D). It is anticipated that D (Compound 2, or Compound B below), as a consequence of its physical properties, will be trapped within the extracellular space of the tumor mass. Thus, when labeled with iodine-131 ( 131 I), a radionuclide that decays by the emission of both a beta particle (E max =610 keV; mean range=467 μm; maximum range=2.4 mm) and photons suitable for external imaging, the entrapped 131 I-labeled D molecules will serve as a means for both assessing tumor-associated radioactivity (planar/SPECT) and delivering a protracted and effective therapeutic dose to the tumor.
[0000]
[0033] Radiolabeled 2-(2′-hydroxyphenyl)-4-(3H)-quinazolinone dyes are employed in the method of the present invention: These classes of compounds contain a hydroxyl group that forms an intramolecular six-membered stable hydrogen bond with the ring nitrogen and hence they are highly water-insoluble in nature. However, addition of a prosthetic group (e.g. phosphate, sulfate, sugars such as galactose or peptide) on the hydroxy group renders the molecule freely water-soluble. Furthermore, the presence of such prosthetic groups makes cell-membranes impermeable to these molecules; they are anticipated to have relatively short biological half-lives in the blood. However, when acted on by the enzyme, the prosthetic group is lost, resulting in the restoration of intramolecular hydrogen bonding, and the molecule becomes water-insoluble and precipitates.
[0034] The procedure for the synthesis of the unsubstituted quinazolinone dye (1, below), is as follows:
[0000]
[0035] 1.3 g anthranilamide (3) and 1.2 g salicylaldehyde (4) were refluxed in methanol. Within 30 minutes, a thick orange precipitate of the Schiff-base (5) was formed. The reaction mixture was cooled in a refrigerator and the product filtered and washed with cold methanol. The precipitate (about 1.5 g) was then suspended in 20 ml ethanol containing p-toluene sulfonic acid and refluxed for 1 hour. The progress of reaction was followed by TLC. The off-white precipitate of dihydroquinazolinone (6) was filtered off and washed thoroughly with cold ethanol. It was then suspended in 12 ml methanol containing 0.6 g dichloro-dicyanobenzoquinone and heated under reflux for 1 hour. The quinazolinone dye product (2) was isolated after cooling the reaction mixture and subsequent filtration. The pale yellow chemical was suspended in diethyl ether and stirred, filtered and washed with ether. To 100 mg of the quinazolinone dye (2) in 1 ml of dry pyridine under nitrogen in an ice bath was added 65 mg (40 μl) of POCl 3 through a syringe. After stirring at this temperature for 30 minutes, it was neutralized by the addition of 116 μl of 30% ammonia. The crude product (1) was evaporated to dryness in rotary evaporator and was partitioned between ethyl acetate and water, the organic layer re-extracted with water, and the combined aqueous extract was back extracted with ethyl acetate. Finally, the product was loaded on to a DEAE Sephacel column (10 ml) pre-equilibrated in bicarbonate form. The column was washed with 20 ml water followed by a stepwise gradient of triethyl ammonium bicarbonate buffer (pH 7.0, 0.1 M to 0.5 M, 25 ml each). Appropriate fluorescent fractions were pooled and lyophilized to dryness (yield 55%). All chemicals were characterized by NMR and elemental analysis.
[0036] In order to make use of the above chemistry for the synthesis of radiolabeled quinazolinones, halogen substituted anthranilamides that are easily converted to the tin prescursors needed for the exchange labeling with radiohalogens were used. Thus, for the synthesis of 5-haloanthranilamides (9) from 5-haloanthranillic acids (7), isatoic anhydrides were used, as shown below.
[0000]
[0037] Such anhydrides are known to react with amines to furnish anthranilamides under certain controlled conditions. Since phosgene gas is not available, reaction conditions were employed using triphosgene which is a solid. 5-Halo-anthranilic acid (bromo- or iodo-) was stirred with equimolar amounts of triphosgene in dry THF at ambient temperature for 1-2 hours. The solution was filtered and diluted with hexane until it became turbid and then stored at −20° C. overnight. The precipitated anhydride (8) was filtered and washed copiously with hexane THF mixture and dried (yield ˜60%). The anhydride (dissolved in THF) was stirred in 1 M aqueous solution of ammonia (containing 1:1 THF) at ambient temperature for 25 minutes. Finally, the organic layer was evaporated under nitrogen and the product (9) was filtered and washed copiously with water followed by acetonitrile and dried in vacuo (yield ˜75%).
[0038] 2-Amino-5-iodobenzoic acid (10) and triphosgene were then dissolved in dry THF and the reaction mixture stirred at room temperature for 1 hour. An off-white precipitate formed and TLC showed that compound 10 is consumed, as shown below. The precipitate was filtered, washed with cold methanol, and crystallized in acetonitrile. 1 H NMR indicated that the spectrum was an iodoisotoic anhydride (11).
[0000]
[0039] A solution of iodoisotoic anhydride (11) was then suspended in THF and cooled in an ice-bath. Aqueous ammonium hydroxide was added dropwise, the reaction mixture was stirred for 15 minutes at 0° C. and 30 minutes at RT, and the solvent was evaporated. The white solid obtained was characterized by 1 H NMR and identified as an iodoanthranilamide (12).
[0040] Next, Iodoanthranilamide (12) and salicylaldehyde were suspended in methanol and refluxed in the presence of catalytic amounts of p-toluene sulfonic acid (TsOH) for 30 minutes. To the pale-yellow precipitate (13) formed, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone was added and the suspension was refluxed for 1 hour. The solid product was filtered, washed with cold methanol, characterized by 1 H NMR, and identified as 2-(2′-Hydroxyphenyl)-6-iodo-4-(3H)-quinazolinone.
Synthesis of Ammonium 2-(2′-Phosphoryloxyphenyl)-6-iodo-4-(3H)-quinazolinone (15)
[0041] In one method, 2-(2′-Hydroxy)-6-iodo-4-(3H)-quinazolinone (14) was added to dried pyridine at 0° C., followed by phosphorus oxychloride. Silica gel TLC indicated that the reaction was completed within 2 min. The reaction solution was neutralized to pH 7.0 by the addition of ammonium hydroxide. The solvent was evaporated and the solid product was suspended in water, filtered, and purified by chromatography. Following elution (stepwise gradient: water followed by acetonitrile-water, 2:1), a yellow solution containing UV-visible product was collected, the solvent was evaporated, and the product was characterized by 1 H and 31 P NMR and identified as compound 15.
[0042] In an alternative method, ammonium 2-(2′-phosphoryloxyphenyl)-6-tributylstannyl-4-(3H)-quinazolinone (17) was dissolved in methanol, and sodium iodide was added followed by hydrogen peroxide. A yellow precipitate formed immediately. The reaction vial was vortex-mixed and incubated for 30 minutes at 37° C. Reversed-phase silica gel TLC showed approximately 50% conversion (solvent: acetonitrile-water, 1:1). The solvent was evaporated and the product purified by chromatography. TLC (solvent: chloroform-methanol, 1:1) showed the same R f value (0.6), and proton and 31 P NMR gave the same spectra as were obtained with the known compound 15 synthesized by the route shown above.
[0000]
[0043] Next, to a dioxane solution containing 14, hexa-n-butylditin and tetrakis (triphenylphosphine) palladium were added, as shown above. The reaction mixture was refluxed for 1.5 hours and progress of the reaction was followed by silica gel TLC (solvent: methylene chloride-ethyl acetate, 9:1) to test for the formation of a more nonpolar product. The solvent was evaporated, and the crude yellow solid was purified on a silica gel column (stepwise gradient: starting with hexane followed by hexane-dichloromethane, 1:1). Following solvent evaporation, a yellow fluorescent solid 2-(2′-Hydroxy)-6-tributylstannyl-4-(3H)-quinazolinone 16 was obtained as identified by 1 H NMR.
[0044] Next, to a stirred solution of 16 in dry pyridine cooled to 0° C., phosphorus oxychloride was added dropwise. The reaction mixture was stirred for 10 min at 0° C. and then quenched by the addition of ammonium hydroxide (Scheme 5). The solvent was evaporated, the crude product redissolved in methanol-acetate (1:1) and purified on a C 18 column (stepwise gradient: water followed by acetonitrile-water going from 30% to 50% acetonitrile). The solvent was evaporated and the nonfluorescent solid Ammonium 2-(2′-Phosphoryloxyphenyl) 6-tributylstannyl-4-(3H)-quinazolinone 17 was obtained as identified by 31 P NMR.
[0045] Next, three Iodo-beads were placed in a reaction vial, followed by 20 μl of 1 μg/μl solution of 17, 30 μl 0.1 M borate buffer (pH=8.3), and Na 125 I (800 μCi/8 μl of 0.1 M sodium hydroxide). After 20 minutes at room temperature, the crude reaction mixture was loaded on a Sep-Pak Plus C 18 cartridge and eluted with 1 ml water and then 2 ml 10% acetonitrile in water. The product 18 was eluted with 20% acetonitrile in water (yield: ˜370 μCi; radiochemical yield: 46%). The radiolabeled product, co-spotted with nonradioactive compound 15 on reversed-phase TLC, showed a single spot on autoradiograph (solvent: acetonitrile-water, 1.5:2). Radiolabeled ( 151 I) Ammonium 2-(2′-Phosphoryloxyphenyl)-6-iodo-4-(3H)-quinazolinone 18 co-injected with 15 into the HPLC showed a single radioactive peak (R f =14 min) which matched the R f value of 15.
[0046] X-Gal (5-bromo-4-chloro-3-indolyl β-D-galactose) is routinely used for the identification of lac + bacterial colonies. The underlying principle is that the colorless X-gal which is freely water-soluble is converted to dark blue colored precipitate upon reaction with b-galactosidase enzyme.
[0000]
[0047] In accordance with the present invention, a bromine atom within X-gal is replaced with a diagnostic/therapeutic nuclide (e.g. Iodine-131, boron-10). For example, an antibody-β-galactosidase immunoconjugate will be administered in the first step. Following its clearance, the water soluble nuclide-labeled X-gal (10) will be injected where at the sites of enzyme action, the X-gal substrate will lose the sugar moiety and the resulting aglycon (11) will precipitate within the targeted tissue. In another embodiment, prosthetic groups other than galactosyl (e.g. phosphate, sulfate, carbonate) as well as nuclides other than iodine-131 and boron-10 may be used.
[0048] When the prodrug ((1) or Compound A), a non-fluorescent, stable, water-soluble compound, is incubated (37° C.) with alkaline phosphatase (ALP), a bright yellow-green fluorescent, clearly visible precipitate is formed whose R f on thin layer chromatography (TLC) corresponds to drug ((2) or Compound B). In order to assess the kinetics of this enzyme-based hydrolysis (i.e. conversion of Compound A to Compound B) at 37° C., Compound A (60 μM) was mixed with 10 units ALP in 0.1 M Tris (pH 7.2) and the reaction kinetics followed over time using a Perkin-Elmer LS50B Luminescence Spectrometer with excitation at 340 nm and emission at 500 nm. There is a rapid increase in fluorescence intensity under these experimental conditions, as shown in FIG. 1 , demonstrating the hydrolysis of Compound A and the formation of Compound B. No fluorescence was observed when the enzyme was heat-inactivated prior to its incubation with Compound A.
[0049] In order to further characterize the 125 I-labeled prodrug, 125 I-labeled Compound A (˜10 μCi/100 μl 0.1 M Tris buffer, pH 7.2) was incubated with 5 units ALP or heat-inactivated (70° C., 2 hours) ALP; the samples were spotted on reversed-phase TLC plates that were then run in acetonitrile-water (1.5:2). Autoradiography demonstrates the complete conversion of 125 I-labeled Compound A to 125 I-labeled Compound B only in the presence of the active enzyme, as shown in FIG. 2 .
[0050] In order to determine blood clearance of AP 125 IQ, mice (n=5/group) were injected i.v. with the radioiodinated prodrug and bled over a 1 hour period, the radioactive content per gram of blood was measured, and the percentage injected dose per gram (% ID/g) calculated. The results as shown in FIG. 3 demonstrate a rapid biphasic blood clearance of radioactivity and a T 1/2β of 51.1±6.8 min.
[0051] In order to assess the chemical nature of the radioactivity in blood (i.e. determine stability of 125 I-labeled Compound A in blood), ethanol was added to the blood samples (collected during the first 40 min), the tubes were centrifuged, and the supernatant was spotted on TLC. The plates were run in acetonitrile-water (1.5:2) and autoradiographed. The results show (i) the presence of a single spot whose R f is the same as that observed with 127 I-labeled Compound A, and (ii) no evidence of free iodine. These data demonstrate the stability of I-labeled Compound A in serum.
[0052] The biodistribution of 125 I-labeled Compound A in normal tissues was also considered. Mice (n=30) were injected i.v. with the radiopharmaceutical (˜5 μCi/100 μl), the animals were killed at 1 hour (n=15) and 24 hours (n=15), and the radioactivity associated with blood, tissues, and organs was determined. As shown in FIG. 4 , (i) the radioactivity in all organs and tissues declined over time; (ii) the radioactivity in the kidneys and urine was high, suggesting that the compound and/or its metabolic breakdown/hydrolysis products were rapidly excreted (since the weight of the thyroid is ˜5 mg, the activity within the thyroid indicates minimal dehalogenation of the compound); and (iii) <20% of the injected dose remained in the body by 24 hours. These results, therefore, demonstrate that 125 I-labeled Compound A and/or its metabolic breakdown/hydrolysis product(s) have a low affinity to normal tissues and that the presence of endogenous ALP leads to minimal hydrolysis of the compound.
[0053] The biodistribution of 125 I-labeled Compound B was also examined in various tissues in normal mice. In these experiments, 125 I-labeled Compound A was synthesized, purified, and incubated at 37° C. in the presence of ALP overnight. TLC demonstrated the complete conversion of 125 I-labeled Compound A to 125 I-labeled Compound B. Mice (n=10) were injected i.v. with 125 I-labeled Compound B (˜5 μCi/100 μl) and killed (n=5) at 1 hour and 24 hours. The 1 hour data, as shown in FIG. 5 , demonstrate the presence of this water-insoluble molecule in all the tissues examined (<15% ID/g). However, by 24 hours ( FIG. 5 ), all tissues and organs (with the exception of minimal activity in the thyroid) were virtually void of radioactivity (<4% of the injected dose remained in the body by 24 hours). These results show that 125 I-labeled Compound B has no avidity for any tissue in the mouse and that the tissue-associated activity seen at 1 hour reflects that within the blood. Since these data seem to argue for the inability of 125 I-labeled Compound B to traverse blood vessel walls and enter into tissues, this water-insoluble molecule if formed within a tissue (e.g. tumor mass) is likely to be retained, i.e. it will not leach back into circulation.
[0054] In order to demonstrate within an animal the conversion of the water-soluble 125 I-labeled Compound A to the water-insoluble 125 I-labeled Compound B, ALP was dissolved in saline (50, 100, 150, 200, 250, 300, 400 units/10 μl) and using a 10-μl syringe, 10 μl enzyme preparation was injected s.c. in the forelimb of Swiss Alpine mice. Five-minutes later, 20 μCi 125 I-labeled Compound A was injected i.v. (tail vein). The animals were killed 1 hour later and the radioactivity in the forelimbs was measured. The results, as shown in FIG. 6 , demonstrate that the radioactive content within the forelimbs of animals pre-injected with ALP increased with enzyme dose and plateaued at the highest concentrations. The fact that these increases were due to the enzymatic action of ALP was ascertained in studies that showed no increase in uptake in the forelimbs of mice pre-injected with heat-inactivated ALP ( FIG. 6 ). These results illustrate the specific dose-dependent accumulation of 125 I-labeled Compound A (more accurately, 125 I-labeled Compound B) within alkaline-phosphatase-containing sites in an animal.
[0055] In order to demonstrate that once formed, the water-insoluble Compound B is retained “indefinitely” within the tissue where it is formed, 125 I-labeled Compound B was dissolved in 100 μl DMSO (under these conditions, 125 I-labeled Compound B is completely soluble in DMSO; however, when 100 μl water are added, a visible precipitate forms immediately that contains 125 I-labeled Compound B radioactivity). Five μl of this solution was injected s.c. into the right forelimb of mice (n=15), followed by 5 μl saline. For comparison, 125 I-labeled Compound A (5 μCi/5 μl saline) was injected s.c. into the left forelimb of the same mice and followed with 5 μl DMSO. The animals were killed after 1 hour, 24 hours, and 48 hours, the radioactivity associated with the forelimbs was measured, and the percentage of radioactivity remaining was calculated (at the 24 hour time point, the biodistribution of radioactivity in various tissues and organs was also determined). The data ( FIG. 7 ) demonstrate that while greater than about 98% of the prodrug 125 I-labeled Compound A had seeped out of the s.c. pocket by 24 hours, 71±5% of the injected precipitable 125 I-labeled Compound B activity remained at the injection site at 24 hours. The biodistribution data ( FIG. 8 ) show that the radioactivity that escaped during the first 24 hours following the s.c. injection of 125 I-labeled Compound B does not localize in any normal tissues within the animal (activity within the thyroid indicates uptake of free iodine). Finally, the results show no change in the radioactivity in the forelimbs of the animals at 24 hours and 48 hours ( FIG. 7 ), thereby indicating that the precipitated 125 I-labeled Compound B is permanently and indefinitely trapped within tissues.
[0056] While this invention has been described in terms of exemplary embodiments, it is not limited thereto. Rather, the appended claims should be construed broadly to include other variants and embodiments of the invention which may be made by those skilled in the art without departing from the scope and range of equivalents of the invention. | The present invention discloses a method for the enzyme-mediated, site-specific, in-vivo precipitation of a water soluble molecule in an animal. The enzyme is either unique to tumor cells, or is produced within a specific site (e.g., tumor) at concentrations that are higher than that in normal tissues. Alternatively, the enzyme is conjugated to a targeting moiety such as an antibody or a receptor-binding molecule. | 0 |
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a polypropylene resin composition and more particularly, to the polypropylene resin composition comprising a high crystalline polypropylene, a polypropylene or polyethylene having low molecular weight, an inorganic filler and an anti-additive. The polypropylene resin of the present invention provides improved heat resistance, impact resistance and scratch resistance, so that it is suitable for substituting conventional polypropylenes used for automotive interior materials having several tens of grades, and further lowers manufacturing cost along with improving productivity and reclamation of used materials.
[0003] Recently, researches have been highly increased to replace engineering resins, i.e. expensive ABS/PC, ABS and PPF, with inexpensive general-purpose resins. For this purpose, a polypropylene resin as one of general-purpose resins was introduced to replace the engineering resin because it has well-balanced molecular structure and provides excellent rigidity and hinge property with low price. However, there are some drawbacks to use such a polypropylene resin in automotive interior materials due to deficient in heat resistance, impact strength and scratch resistance, resulting in the production of inferior goods having thermal deformation and scratches and the formation of cracks by external impact. And further, molecular weight remarkably decreases due to the thermal deformation during an injection molding process at a temperature of over 280° C. Such problems indicate that use of the conventional polypropylene resins is limited for high functionalities of automotive interior parts due to its inferior properties. Since conventional polypropylene resins used for automotive interior materials require several tens of grades to satisfy the qualities and physical properties, color matching becomes poor and a resin inside an injection mold has to be changed with changing of a different grade resin during the process, resulting in deterioration of processability and efficiency and rising manufacturing cost. In terms of reclamation, the recycling cost becomes high and the physical properties of reclaimed products become poor, so that it deteriorates its commercial value.
[0004] Recently, Toyota motor company has developed a polypropylene resin which integrates polypropylene resins graded into several tens to one grade for interior automotive materials. This development stands high in estimation because a separation process according to the grade becomes unnecessary, it lowers the manufacturing cost, the physical properties of reclaimed products are improved and commercial value becomes better.
SUMMARY OF THE INVENTION
[0005] Consequently, an object of the present invention is to provide a polypropylene resin composition comprising a high crystalline polypropylene, a polypropylene or polyethylene with low molecular weight, an inorganic filler and an anti-additive to have advantages over the above-mentioned polypropylene resins in that it exhibits excellent impact strength, heat resistance by improving heat distortion temperature and durability to minimize scratches and cracks, it lowers the manufacturing cost, it enhances processability by integrating graded polypropylene resins to one, and it improves color matching and physical properties of reclaimed materials, so that it can be suitable for interior automotive pillar and trim parts.
DETAILED DESCRIPTION OF THE INVENTION
[0006] The present invention provides a polypropylene resin composition comprising 50-90wt. % of a high crystalline polypropylene, 5-50wt. % of polypropylene or polyethylene having low molecular weight, 0.1-3wt. % of an inorganic filler, and 0.1-0.5 wt. % of an anti-additive.
[0007] The present invention is described in detail as set forth hereunder.
[0008] The present invention is characterized by a polypropylene resin composition comprising a high crystalline polypropylene as one of components selected from the group consisting of a high crystalline propylene homopolymer having propylene monomers as a main component, an ethylene-propylene block copolymer having ethylenes and a mixture thereof.
[0009] The high crystalline polypropylene used in the polypropylene resin composition provides excellent durability and scratch resistance due to high crystallinity. The high crystalline polypropylene used in the present invention has pentad fraction (% mmmm) measured by 13 C-NMR higher than 97% and melt index of 0.5-50 g/10 min. The high crystalline polypropylene is used in 50-90 wt. % of the entire polypropylene resin composition, preferably in 70-80 wt. %. If the content exceeds 90 wt. %, the impact resistance and scratch resistance become degraded because it requires high fluidity having a melt index of over 12; otherwise if it is below 50wt. %, the scratch resistance and modulus of bending elasticity are degraded. The high crystalline ethylene-propylene block copolymer of the present invention is preferred to contain 3-10 wt. % of an ethylene content.
[0010] Polypropylene or polyethylene having low molecular weight of the present invention is used to provide better flowabilty of resins during molding process and complement poor impact strength at a low temperature. The polypropylene can be propylene homopolymer, ethylene-propylene block copolymer, or a mixture thereof having a melt index of 0.5-50 g/10 min. A polypropylene having low molecular weight is used to provide improved impact strength of the resultant polypropylene resin composition in case of low melt index and improved flowability in case of high melt index. The polypropylene having low molecular weight is used in 5-50 wt. % of the entire polypropylene resin composition, preferably in 20-30 wt. %. If the content exceeds 50 wt. %, the impact resistance and scratch resistance become degraded; otherwise if it is below 5 wt. %, the flowability becomes inferior.
[0011] Polyethylene of the present invention is used to complement poor impact strength of the polypropylene resin composition at a low temperature and is preferred to have a melt index of 1-25 g/10 min and a specific gravity of 0.915-0.964. The polyethylene is used in 5-50 wt. % of the entire polypropylene resin composition, preferably in 20-30 wt. %. If the content exceeds 50 wt. %, the scratch resistance becomes degraded; otherwise if it is below 5 wt. %, the impact strength becomes inferior.
[0012] An inorganic filler as another component of the polypropylene resin composition acts as a nucleating agent to improve scratch resistance and rigidity and provides lower manufacturing cost and crosslinking effect. Particles of the inorganic filler are preferred to have spherical shape and small size on the purpose of increasing surface tension of particles to improve rigidity of the composition. The average particle size is preferred to be in the range of 1-4 μm. If the particle size is larger than 4 μm, cracks can be produced around the particles and elongation becomes inferior; otherwise if it is smaller than 1 μm, distribution of the resin may be degraded with conventional compounding method. Said inorganic filler is used in the range of from 0.1 to 3 wt. % to the entire polypropylene resin composition. When it is less than 0.1 wt. %, it is not enough to act as a nucleating agent to improve scratch resistance and rigidity. On the other hand, when it is more than 3 wt. %, the elongation becomes inferior. Said inorganic filler can be talc, wollastonite, or a mixture thereof.
[0013] An anti-additive of the present invention is used to provide excellent fowability and scratch resistance of the polypropylene resin composition of the present invention. The anti-additive can be fatty acid, fatty acid amide, monoester or glycerin mono-stearate containing 40-95 wt. % of a mixture thereof. Said anti-additive is used in the range of from 0.1 to 0.5 wt. % to the entire polypropylene resin composition. When it is less than 0.1 wt. %, flowability becomes degraded. On the other hand, when it is more than 0.5 wt. %, scratch resistance does not increase further.
[0014] Besides these components, an elastomer may be incorporated in the range of 1-2 wt. %, if desired. Examples of the elastomer are ethylene-propylene elastomer (EPR), ethylene-propylene-diene elastomer (EPDM), polyethylene prepared using a metallocene catalyst, or a mixture thereof. Other additives, used by one having ordinary skill in the art, such as an anti-oxidant, a heat stabilizer, and a TV stabilizer may be arbitrarily incorporated in an appropriate content not to obstruct the above-mentioned object of the present invention.
[0015] The polypropylene resin composition of the present invention is prepared by mixing and compounding a mixture of a high crystalline polypropylene, a polypropylene or polyethylene having low molecular weight, an inorganic filler, an anti-additive, and other additives and the prepared polypropylene resin composition is then palletized and molded by the means of injection molding to produce desired automotive parts such as pillar and trim parts. Therefore, use of the polypropylene resin composition of the present invention instead of conventional polypropylene resin graded to several tens improves sharply a manufacturing process and controlling the resin, color matching and physical properties of reclaimed materials with lowering the manufacturing cost.
[0016] Hereunder is given a more detailed description of the present invention using examples. However, it should not be construed as limiting the scope of this invention.
EXAMPLES 1-3
[0017] A mixture of high crystalline polypropylene, polypropylene or polyethylene having low molecular weight, inorganic filler and anti-additive was mixed with listed amount and ratio in Table 1 and compounded at 180-230° C. The resulting mixture was melt-kneaded with twin-screw extruder, palletized, and molded by injection molding machine to obtain test specimen.
TABLE 1 Example (wt. %) Composition 1 2 3 High crystalline polypropylene 1) 79.3 50 89.3 Propylene homopolymer 20 2) 49.2 3) — Ethylene-propylene block copolymer 4) — — 10 Inorganic filler 5) 0.3 0.5 0.4 Anti-additive 6) 0.4 0.3 0.3
[0018] The ethylene content contained in high crystalline polypropylene is measured by means of using FT-IR spectrometer.
[0019] Experimental example
[0020] Physical properties of the polypropylene resin composition prepared from Examples 1-3 were tested by the following method. The result is shown in Table 2.
[0021] [Test Method]
[0022] A. Melt index (MI, g/10 min): Tested with ASTM D1238 (230° C./2.16 kg)
[0023] B. Special gravity (g/ml): Tested with ASTM D791
[0024] C. Tensile strength (kg/cm 3 ) and Elongation (%): Tested with ASTM
[0025] D638 (thickness of the specimen 3 mm, 23° C.)
[0026] D. Modulus of bending elasticity (kg/cm 3 ): Tested with ASTM D79 (thickness of the specimen 3 mm, 23° C.)
[0027] E. IZOD Impact strength (kg·cm/cm 2 ): Tested with ASTM D256 (thickness of the specimen 3 mm, 23° C.)
[0028] F. Thermal deformation temperature (°C.): Tested with ASTM D648 (4.6 kg loaded, thickness of the specimen 3 mm)
[0029] G. Lead hardness of pencil: Tested with JIS K-0202
TABLE 2 Example Items 1 2 3 Melt index (MI, g/10 min) 12.1 13 12.2 Special gravity (g/ml) 0.91 0.91 0.91 Tensile strength (kg/cm 3 ) 344 350 332 Elongation (%) >500 500 >500 Modulus of bending elasticity 22,117 20,412 21,034 (kg/cm 3 ) IZOD Impact strength (kg.cm/cm 2 ) 12.1 10.2 13.6 Thermal deformation temperature 137 138 136 (° C.) Lead hardness of pencil 3B 3B 3B
[0030] As shown in table 2, the polypropylene resin composition of the present invention provides superior scratch resistance, impact strength and heat resistance to those of the conventional polypropylene resin compositions.
[0031] According to the present invention, as described above, the polypropylene resin composition has sufficient scratch resistance, impact strength and heat resistance, so that it has excellent properties satisfactorily to fit for use in interior automotive parts such as pillar and trim parts. | The present invention relates to a polypropylene resin composition and more particularly, to the polypropylene resin composition comprising a high crystalline polypropylene, a polypropylene or polyethylene having low molecular weight, an inorganic filler and an anti-additive. The polypropylene resin of the present invention provides improved heat resistance, impact resistance and scratch resistance, so that it is suitable for substituting conventional polypropylenes used for automotive interior materials having several tens of grades, and further lowers manufacturing cost along with improving productivity and reclamation of used materials. | 2 |
FIELD OF THE INVENTION
The present invention relates to systems and methods for managing data. In particular, but not by way of limitation, the present invention relates to systems and methods for categorizing, collecting and/or analyzing customer service data.
BACKGROUND OF THE INVENTION
Customer service often requires quick, consistent responses to customer inquiries. In the not so distant past, live service agents responded to most customer inquires by phone. Phone responses are extremely expensive, and with the spread of the internet, live agents began to respond to customer inquiries by cheaper methods such as email and chat programs.
Live agents, whether responding by phone, email or chat program, remain important for many businesses. Companies seeking to further reduce their costs, however, replaced or supplemented live agents with automated systems such as virtual agents and interactive voice response (IVR) systems. Automated systems respond to routine customer inquiries based on a decision tree and/or active logic. These systems are often referred to as “response systems.”
All of these different response systems generally generate some performance metrics by which they can be evaluated. For example, a phone response system can report the number of calls received, average number of minutes required to respond to each call, number of calls abandoned before being reached, etc. Other response systems generally report similar metrics.
Different response systems are generally not integrated, and the different reporting metrics are integrated poorly, if at all. A customer with an email response system, a voice response system, and an automated agent could receive three different sets of metrics and may have no way to evaluate the combined performance of all three systems. Further, these disparate response systems do not enable a consistent response strategy for addressing user inquiries. A phone operator, for example, could generate a different response to a particular inquiry than would an automated system. Such response inconsistencies make integrating metrics from different response systems difficult.
Although present response systems are functional, they are not satisfactory. A system and method are needed to address the shortfalls of present technology and to provide other new and innovative features. For example, systems and methods are needed to better provide an overall, or holistic view, of a company's interaction with its customers. Similarly, a system and method are needed to provide a consistent response strategy across all types of response systems.
SUMMARY OF THE INVENTION
One embodiment of the technology disclosed herein provides an overall, or holistic view, of an enterprise's interaction with its customers. These embodiments can also provide a holistic view of other types of interactions. In one particular embodiment, a system collects and aggregates information related to user inquiries and/or responses generated by different types of response systems. Such an embodiment could collect data about phone response system activities and aggregate that information with data about an automated response system activities. Other embodiments collect and aggregate information related to customer information, contact resolutions and other information. Other embodiments of the disclosed technology generate reports based on aggregated information and/or generate recommendations to address problems with the individual response systems or the overall strategy for responding to customer inquiries.
These and other embodiments are more fully described in the Detailed Description section. It is to be understood, however, that there is no intention to limit the invention to the forms described in this Summary of the Invention or in the Detailed Description. One skilled in the art can recognize that there are numerous modifications, equivalents and alternative constructions that fall within the spirit and scope of the invention as expressed in the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
Various objects and advantages and a more complete understanding of the present invention are apparent and more readily appreciated by reference to the following Detailed Description and to the appended claims when taken in conjunction with the accompanying Drawings wherein:
FIG. 1 is a block diagram of a system for responding to and analyzing customer inquiries;
FIG. 2 is a block diagram of another system for responding to and analyzing customer inquiries;
FIG. 3 is a flowchart of one method for collecting customer inquiry information from different response systems;
FIG. 4 is a flowchart of one method for analyzing customer inquiry information;
FIG. 5 is a chart illustrating one method for presenting information about customer inquiries;
FIG. 6 is a flowchart of one method for generating an overlaid contact center graph; and
FIG. 7 is another chart illustrating a method for presenting information about customer inquiries.
DETAILED DESCRIPTION
Referring now to the drawings, where like or similar elements are designated with identical reference numerals throughout the several views, and referring in particular to FIG. 1 , it illustrates a block diagram of a system 100 for responding to and analyzing customer inquiries. It should be noted, that “customer” can refer to any user or system and is not limited to a party making a commercial transaction. This embodiment of the invention includes a response center 105 coupled to a plain old telephone switch (POTS) 110 and to a network 115 such as the Internet. Through these two networks, customers 120 can communicate with the response center 105 .
This version of the response center 105 includes several individual response systems: phone 125 , chat 130 , email 135 , automated agent 140 , and interactive voice response (IVR) 145 . The response center 105 could also include other systems for communicating with customers or could include fewer response systems than illustrated.
Each response system can retrieve a recommended response to a customer inquiry from the global knowledge database 150 , which can include decision trees and/or logic for compiling responses to customer inquiries. The decision trees/logic can be used by all types of response systems. If necessary, a response system can also retrieve customer data from the customer information database 155 or other data from a third party database (not shown) to generate its responses. For example, when the customer 120 sends an email requesting information on how to cancel an order, a live customer agent at the email response center can search the global knowledge database 150 for the proper response. The agent can then include that response, or at least some portion of the response, in the email to the customer 120 . If the same request for information originated by phone, the phone agent could pull the same response, or a similar response template, from the global knowledge database 150 and use it as a transcript for talking with the customer 120 . Thus, the same customer inquiry can be answered generally in the same way regardless of the customer's method of communicating the inquiry.
Response information included in the global knowledge database 150 can be categorized and/or coded to aid in retrieval and identification of proper responses and in record accumulation. The order cancellation response, for example, could be coded as response number “29.” Each of the response systems, regardless of type, can generate an order cancellation response based on response number “29.” Further, when any response system generates an order cancellation response, the response system can provide the proper code, “29,” to the analysis engine or analysis database 160 .
When a response system provides a response to a customer 120 , it also stores an indication of the generating response system in the analysis database 160 . For example, when the automated agent 140 generates an order cancellation response, it can store a “29” in the analysis database 160 along with an identifier for the automated agent. Other data can also be stored in the analysis database 160 , including time stamps, network statistics, user data, etc.
In one embodiment, the analysis engine 165 can retrieve data from the analysis database 160 and report on the activities of the various response systems. One embodiment of such a report is shown in FIG. 5 , which is described in detail below. Typical reports illustrate the number or percentage of responses generated by each individual response system for each response or response category. For example, a report could indicate that two number “29” responses were generated by the response center 105 and that one of those two responses was generated by the automated agent system 140 and the other by the phone response system 125 .
Referring now to FIG. 2 , it is a block diagram of another system 170 for responding to and analyzing customer inquiries. This embodiment is similar to the embodiment shown in FIG. 1 except that it includes distributed response systems that are not necessarily integrated. Even if not integrated, each response center can draw its responses or template for responses from the global knowledge database 150 and store indications of generated response and the generating response systems in the analysis database 160 .
Referring now to FIG. 3 , it is a flowchart of one method for collecting customer inquiry information from different response systems. In this embodiment, a response system initially receives a customer inquiry. (Block 175 .) The customer can originate the inquiry through a phone call, an email, a link activation, etc. Once the inquiry has been received, the response system determines the proper response and provides it to the customer. (Blocks 180 and 185 .) If the response system is staffed with live agents, the live agents are generally responsible for determining the proper response using, for example, a decision tree or template included in the global knowledge database. If the response system is an automated response system, such as a virtual agent or IVR system, the computer is responsible for using the global knowledge database to respond to the user inquiry. Manual intervention is not generally necessary.
For each response to a customer inquiry, the response identifier is determined and stored in, for example, the analysis database. (Blocks 190 and 195 .) An indication of the response system that generated the response can also be stored with the response identifier. In some embodiments, the indication can be as simple as increasing a counter associated with both the response and response system.
Referring now to FIG. 4 , it is a flowchart of one method for analyzing customer inquiry information. As described with relation to FIG. 3 , categorization information related to a generated response is received and stored in a database, typically the analysis database. (Blocks 200 and 205 .) This information, as previously described, includes both the response identifier and an indication of the response system. Other information related to the response can also be collected. For example, customer identifiers, customer activities, type of customer, time of day, and lapsed time for generating the response can be collected. This information can be aggregated together or used alone to evaluate the performance of a particular response system or the overall response center. (Blocks 210 and 215 .) In yet another embodiment, data related to the customer inquiries can be stored and used to evaluate performance.
Referring now to FIG. 5 , it is a chart 220 illustrating one method for presenting information about customer inquiries and responses. This chart includes three overlaid pie charts. The inner chart illustrates a broad category of customer responses. The middle chart illustrates a subcategory of the customer responses shown in the inner chart, and the outer chart indicates the response system used to generate the customer responses corresponding to the middle chart. For example, the inner chart includes a category of customer responses entitled “order status.” The “order status” category includes two subcategories: “modify” and “shipping information.” The outer chart illustrates which response systems generated responses for those subcategories and how many responses were generated by each. For example, this chart illustrates that for the “shipping information” subcategory, the email and phone response systems generated responses and that the email response system generated about twice as many responses as did the phone system.
Using this type of overlaid graph, an analyst can determine what type of issues customers are raising and how those issues are being resolved. In particular, an analyst can determine if particular categories of questions arise often or if a particular category of questions is resolved too often by expensive means such as the phone response system.
Each portion of the overlaid graph can link to other graphs or additional information. For example, if an analyst selected the “order status” category in the inner chart, then a new graph could be displayed showing more detail. A typical graph is shown in FIG. 7 . Additionally, selecting a category could cause hyperlinks, flat files, costs, images, or tables to be displayed. In other embodiments, the “email” area for a particular subcategory can be linked to additional data such as receipt time, average response time, repeat users, etc.
Referring now to FIG. 6 , it is a flowchart of one method for generating an overlaid contact center graph. This method involves identifying categories and subcategories of customer contacts. (Blocks 225 and 230 .) In some embodiments, multiple levels of subcategories can be identified and incorporated into the graph. The graphs in FIGS. 5 and 7 , however, only show one level. Other levels would be illustrated by additional rings in the graphs.
The analysis engine, or some other logic system, can retrieve information from each response system relating to the number of responses provided for each category and/or subcategory. (Block 235 .) For example, the analysis engine can collect all data related to responses in the category “order status,” subcategory “modify,” and further subcategory “vendor 1 .” (Shown in FIG. 7 .) The analysis engine could also retrieve information relating to which response system, phone or email for example, generated the responses. Using the retrieved data, the analysis engine can generate an overlaid contact center graph. (Block 240 .)
The overlaid graph and/or the underlying data can be used to generate recommendations to improve the response center or individual response systems. (Block 245 .) Three typical recommendations include: change a business process, enhance the handling of a customer contact, and automate the response to the customer. Notably, one embodiment of the present invention provides an iterative method for improving a response center. For example, if the reports indicate that a particular inquiry is being too often handled by email, the automated agent could be modified to better handle that category of inquiry, hopefully reducing overall costs.
In conclusion, the present invention provides, among other things, a system and method for improving response centers. Those skilled in the art can readily recognize that numerous variations and substitutions may be made in the invention, its use and its configuration to achieve substantially the same results as achieved by the embodiments described herein. Accordingly, there is no intention to limit the invention to the disclosed exemplary forms. Many variations, modifications and alternative constructions fall within the scope and spirit of the disclosed invention as expressed in the claims. | Embodiments of the technology disclosed herein provides an overall, or holistic view, of an enterprise's interaction with its customers. These embodiments can also provide a holistic view of other types of interactions. In one particular embodiment, a system collects and aggregates information related to user inquiries and/or response generated by different types of response systems. Such an embodiment could collect data about phone response system activities and aggregate that information with data about automated response system activities. Other embodiments collect and aggregate information related to customer information, contact resolutions and other information. Other embodiments of the disclosed technology generate reports based on aggregated information and/or generate recommendations to address problems with the individual response systems or the overall strategy for responding to customer inquiries. | 7 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a modular drilling or workover rig substructure which may be transported to and from a rig site without entirely dismantling the substructure. In particular, the present invention is directed to a modular drilling rig substructure that may be transported to and from a rig site with various drill floor equipment and hand rails remaining in place and that minimizes liquid discharge by providing an integrated containment and drainage system.
2. Prior Art
A drilling rig substructure is one important component of a drilling or workover rig. Typically, a drilling rig substructure includes a raised platform or drilling floor which is above the level of a main deck or cellar deck and above the level of a well head, a blowout preventer and other equipment. An upstanding mast is connected to a floor of the rig and is often supported by the substructure. The mast may extend from 30 to 60 meters so that a substantial amount of weight is supported by the substructure.
The drilling rig substructure includes certain drilling floor equipment and supports personnel for various operations such as connecting and disconnecting pipe sections. Examples of equipment on the drilling floor include rotary tables, power tong apparatus, pipe handling systems, hydraulic winches, powered hoists and controls operated by personnel. Additionally, a V-door ramp may extend from the floor for movement of tubulars and equipment.
It is often necessary to move a drilling or workover rig, including all of its equipment, from one site to another. Traditionally, a rig substructure is assembled or rigged up by assembling the various component pieces of the substructure. For example, a framework is assembled and a plurality of floor panels are put in place to support the equipment and personnel on the drilling floor. While the floor panels are adequate for the purpose of support, they typically do not form a liquid-tight floor section. Accordingly, oil, liquids or debris may run off in the surrounding area. Increasingly, it is desirable to contain any such run-off.
Conversely, the drilling rig substructure is typically disassembled or rigged down by disassembling the various component pieces of the substructure. The various components are then transported to an alternate rig site and the entire process is again repeated.
In the past, various attempts have been made to place various equipment together in modular arrangements. For example, Bierscheid, Jr. (U.S. Pat. No. 4,899,832) discloses a modular drilling apparatus with a combined mast and drilling platform to facilitate assembly and disassembly of the drilling rig. Bierscheid, Jr. does not, however, provide a modular substructure.
It would be advantageous to provide a modular substructure apparatus and method wherein modular components could be moved to and from a rig site by trailer or other vehicle.
It would be advantageous to provide a modular substructure apparatus and process wherein various drill floor equipment and hand rails could remain in place during rig up, during rig down and during transportation operations.
It would also be desirable to provide a modular substructure apparatus and method to facilitate zero liquid discharge from the drill floor by providing an integrated substructure floor and drainage system.
It would be desirable to provide a modular substructure apparatus and method eliminating the requirement of a crane or a gin pole to assemble or rig up and to disassemble or rig down the substructure at a rig site.
It would be advantageous to provide a modular substructure apparatus and method wherein various structural, hydraulic and piping connections could be made at ground level prior to raising the drilling floor to its upstanding, use position.
It would be advantageous to provide a modular drilling rig substructure wherein component sections are joined by connectors not exposed to hook, rotary or set back live loads.
It would be advantageous to provide a modular drilling rig substructure having a drilling floor movable between a lowered, transportation position and an upstanding use position wherein the drilling floor remains parallel to a base at all times.
SUMMARY OF THE INVENTION
The present invention is directed to a modular drilling rig substructure which is comprised of three discreet, modular components—driller side substructure section, center substructure section and an off driller side substructure section. The center section is juxtaposed and lies between the driller side substructure section and the off driller side substructure section.
The driller side substructure section includes a base having a lower skid suitable to be lowered on, loaded off and transported from a trailer or other vehicle. Parallel to and above the base is a floor frame assembly. Pivotally connected between the base and floor frame assembly are a pair of front legs, a pair of middle legs and a pair of rear legs. The front legs, middle legs and rear legs are each pivotally connected to the base. Likewise, the front legs, the middle legs and the rear legs are pivotally connected to the floor frame assembly of the driller side substructure section. Accordingly, the floor frame assembly, the base, the front legs, and the rear legs form a parallelogram. The floor frame assembly can thus move between an upright, in-use position and a lower position parallel to and adjacent to the base for transportation.
The off driller side substructure section operates in the same manner. The off driller side substructure section includes a base, a pair of front legs, middle legs and a pair of rear legs. The front legs, middle legs, and rear legs are each pivotally connected to the base. Likewise, the front legs, middle legs, and rear legs are each pivotally connected to a floor frame assembly of the off driller side substructure section. Accordingly, the floor frame assembly, the base, the front legs and the rear legs together form a parallelogram. In order to assemble a drilling or workover rig substructure, the driller side substructure section and the off driller side substructure section are each transported to a selected rig site in a lowered position. The base of the driller side substructure section is adjacent a drawworks while the base of the off drillers side substructure section is adjacent the drawworks. The driller side substructure section and the off driller side substructure section are parallel to each other and are also spaced apart from each other. Once the off driller side section and the driller side section are in place, the center substructure section is transported and brought to the rig site. The center substructure section is transported on the trailer of a truck with the space between the two side sections being wider than the width of the truck. Accordingly, the truck can back up between the side sections to deposit the center section in place. Thereafter, the center substructure section is pinned to the driller side substructure section and the center section is pinned to the off driller side substructure section.
An hydraulic cylinder between the base and floor assembly on the driller side substructure section is utilized to raise the substructure into the upright, use position. Likewise, an hydraulic cylinder between the base and floor assembly of the off driller side substructure section is utilized to raise the substructure to the upright, use position. The center substructure section is connected to the side sections so that it is raised or lowered along with the side sections. The fully assembled substructure forms an integrated floor with a railing surrounding the drill floor. The drill floor forms a zero discharge floor having a perimeter drain system. Located on the drill floor are various pieces of equipment which may remain in place not only in the use position but also during disassembly and while in the transportation position.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1A is a drillers side elevational view of a modular drilling rig substructure constructed in accordance with the present invention in the use position, FIG. 1B is in the lowered position, and FIGS. 1C and 1D are in intermediate positions;
FIG. 2 is a sectional view of the modular drilling rig substructure in the use position taken along section line 2 — 2 of FIG. 1 with front legs of the substructure also shown in dashed lines in the lowered position;
FIG. 3 is a top view showing the component sections of the drilling rig substructure in the lowered position with portions of the flooring removed for clarity;
FIG. 4 is a top view of the assembled rig substructure in the use position with portions of the flooring removed for clarity;
FIG. 5 is a front view of the rig substructure in the upright use position;
FIG. 6 is a sectional view of the rig substructure taken along section line 6 — 6 of FIG. 1 ;
FIG. 7 is an enlarged view of the portion shown in FIG. 6 ;
FIG. 8 is a top view of the connection shown in FIG. 7 ;
FIG. 9 is an enlarged view of the connection shown in the dashed line circle in FIG. 1 ,
FIG. 10 is a top view of the connection shown in FIG. 9 , and
FIG. 11 is a side view of the connection shown in FIG. 9 ;
FIG. 12 is an enlarged view of the connection shown in the dashed line circle in FIG. 1 ,
FIG. 13 is a top view of the connection shown in FIG. 12 , and
FIG. 14 is a side view of the connection shown in FIG. 12 ; and
FIG. 15 is a top view of the assembled rig substructure showing various equipment on the drill floor.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The embodiments discussed herein are merely illustrative of specific manners in which to make and use the invention and are not to be interpreted as limiting the scope of the instant invention.
While the invention has been described with a certain degree of particularity, it is to be noted that many modifications may be made in the details of the invention's construction and the arrangement of its components without departing from the spirit and scope of this disclosure. It is understood that the invention is not limited to the embodiments set forth herein for purposes of exemplification.
Referring to the drawings in detail, FIG. 1A is a side elevational view of a modular drilling rig substructure 10 constructed in accordance with the present invention. As seen in FIG. 1 , the rig substructure is an upright, in use and fully assembled condition and in place adjacent to a drawworks 12 . A mast (not shown) would be brought to and installed on the rig substructure 10 .
The rig substructure 10 includes a safety railing 16 surrounding a drill floor 18 . An opening in the railing 16 accommodates a personnel trailer, driller's cabin, or “dog house” for drilling rig personnel. The driller's cabin may be supported by the drill floor of the substructure or may have its own support assembly depending on the particular arrangement. Accordingly, the view in FIG. 1A is from the drillers side view. The opposite side is known as and will be described herein as the off driller side.
The drawworks 12 itself may be modular and reside on a skid to be moved to and from a rig site. The substructure is comprised of three discreet, modular components—a driller side substructure section 20 visible in FIGS. 1A , B, C and D, a center substructure section 22 partially visible in FIG. 1A , and an off driller side substructure section 24 (not visible in FIGS. 1A , B, C and D). The center section 22 is juxtaposed and lies between the driller side substructure section 20 and the off driller side substructure section 24 .
As seen in FIG. 1A , the driller side substructure section 20 includes a base 30 having a lower skid suitable to be loaded on, loaded off and transported on a trailer or other vehicle. Parallel to and spaced above the base 30 is a floor frame assembly 32 . Pivotally connected between the base 30 and floor frame assembly 32 are a pair of front legs 34 , a pair of middle legs 36 and a pair of rear legs 38 . The front legs 34 , middle legs 36 and rear legs 38 are each pivotally connected to the base 30 . Likewise, the front legs 34 , middle legs 36 , and rear legs 38 are each pivotally connected to the floor frame assembly 32 of the driller side substructure section 20 . Accordingly, the floor frame assembly 32 , the base 30 , the front legs 34 and rear legs 38 form a parallelogram. The floor frame assembly 32 is capable of moving between an upright, in-use position shown in FIG. 1A and a lower position parallel and adjacent to the base for transportation shown in FIG. 1 B. FIGS. 1C and 1D illustrate intermediate positions between the lowered position in 1 B and upright position in FIG. 1 A.
The off driller side substructure section 24 operates in the same manner.
FIG. 2 is a sectional view taken along section line 2 — 2 of FIG. 1 A. As seen in FIG. 2 , the driller side substructure section 20 and the off driller side substructure section 24 are parallel to each other and also spaced apart from each other. The space therebetween receives the center substructure section 22 which has been removed for clarity and is not seen in FIG. 2 . Driller side substructure section 20 includes rear legs 38 , middle legs 36 and front legs 34 . When the substructure 10 is rotated from the upright, use position shown in FIGS. 1A and 2 to the lowered transportation position show in FIG. 1B , the front legs 34 will move and rotate so that they are in the position shown in dashed lines 34 ′.
Likewise, the off driller side substructure section 24 includes a base 42 , a pair of front legs 48 , middle legs 46 and a pair of rear legs 44 . The front legs 48 , middle legs 46 , and rear legs 44 are pivotally connected to the base 42 . When the substructure 10 is rotated from the upright, use position shown in FIGS. 1A and 2 to the lowered position shown in FIG. 1B , the front legs 48 will move and rotate so that they are in the position shown in dashed lines 48 ′.
A base brace 50 between the base 30 of the driller side substructure section and the base 42 of the off driller side substructure section is visible. The brace 50 is pivotally connected to the base 42 of the off driller side substructure section 24 and moves radially. A diagonal brace 52 between the front legs 34 and 48 and a diagonal brace 54 between the rear legs 38 and 44 may be provided for stabilization.
In order to assemble a drilling rig or workover rig substructure 10 , the driller side substructure section 20 and the off driller side substructure section 24 are each transported to a selected rig site in a lowered position as shown in FIG. 3 . The base 30 of the driller side substructure section is adjacent the drawworks 12 while the base 42 of the off driller side substructure section is adjacent the drawworks 12 . Once the off driller side section 24 and the driller side section 20 are in place, the center substructure section 22 is ready for installation. In one arrangement shown in FIG. 3 , the center substructure section 22 is transported on a trailer of a truck with the space between the two side sections being wider than the width of the truck. Accordingly, the truck can back up between the drillers and off driller side sections to deposit the center substructure section in place.
For clarity, drilling floor panels 56 have been partially cut away in order to view the framework for the floor frame assembly 32 of the driller side substructure and the floor of the off driller side section.
FIG. 4 illustrates a subsequent sequence in the process whereby the center subsection 22 has been brought into place and secured to the drillers side and off drillers side sections, as will be described herein.
Intersecting dashed lines 58 depict the center line of the wellhead over which the substructure 10 is installed.
As seen in FIG. 4 , the center substructure section 22 includes a frame forming a skid 60 to be received on a trailer for transportation. In one arrangement to assemble, a tandem-type trailer will move the center section 22 between the side sections and, with a rolling tail board, tip the center section to set the center section in place.
FIG. 5 illustrates a front view of the substructure 10 while FIG. 6 illustrates a rear view of the substructure in the upright, use position. In FIG. 5 , the pair of front legs 34 of the driller side subsection and the pair of front legs 48 of the off driller side subsection are visible. Cross bracing 64 between the pairs of front legs may be utilized. An hydraulic cylinder 70 between the base 30 and floor assembly 32 of the driller side substructure section 20 is utilized to raise the drill floor into the upright, use position. Likewise, an hydraulic cylinder 72 between the base 42 and the floor assembly of the off driller side section 24 is utilized to raise the floor to the upright, use position. The cylinders 70 and 72 are powered by the hydraulic power system of the rig. The center section is connected to the side sections so that it is raised or lowered along with side sections.
The pair of rear legs 38 of the drillers side substructure section and the pair of rear legs 44 of the off driller side substructure section are visible in FIG. 6 .
FIG. 7 illustrates the connection between center section 22 and the side substructure sections, an enlarged view of the portion shown in the dashed line circle in FIGS. 5 and 6 . The center section 22 includes a protrusion in the form of a tube 74 which extends along each side of the center section 22 . The side substructure section includes an L-shaped shelf 76 . The tube 74 and, in turn, the center section 22 rests upon the shelf. Accordingly, the center section 22 is supported on the shelves of the driller and off driller side substructure sections.
FIG. 8 is a top view of the connection shown in FIG. 7. A set of pins 78 extends through the tube 74 and through the shelf 76 in order to secure the center section to the side sections. While FIGS. 7 and 8 illustrate the connection between the center section and the off driller side subsection, a similar arrangement is provided to connect the center section with the drillers side section.
FIG. 9 illustrates an enlarged view of the pivotal connection between the base 30 of the drillers side section and the rear leg or legs 38 . A stop 80 extending from the base 30 restricts the rear leg 38 from moving past the vertical position. The rear legs 38 move about a hinge 82 between the upright position shown in FIGS. 9 , 10 and 11 and a lower position. It will be observed that the pin does not carry any of the load of the substructure while in the upright use position.
FIG. 12 shows an enlarged view of the pivotal connection between the base 30 of the drillers side subsection and the front legs 34 .
FIG. 13 is a top view of the pivotal connection shown in FIG. 12 while FIG. 14 is a side view of the connection shown in FIG. 12 . The front legs 34 moves about hinge 90 so that the front legs 34 move between the upright position shown in FIGS. 12 , 13 and 14 and a lowered, transportation position illustrated by the dashed lines in FIG. 12 . The front legs terminate in a shear block which provides a contact with a base box pin plate on the base 30 to provide a significant mating area. It will be observed that the pin does not carry any of the load of the substructure while in the upright position.
FIG. 15 illustrates a top view of the fully assembled substructure with a railing 16 surrounding the entire drill floor 18 . As the substructure sections have integrated floors, which are not dismantled during rig up or rig down, the drill floor 18 forms a zero discharge floor having a perimeter drain system. On the drill floor are various pieces of equipment which remain in place not only in the use position but also while in the transportation position. For example, winches 92 , stand pipe manifold 94 , rotary table 96 , wire line unit 98 and shoes 100 and 102 for the mast are visible.
Hydraulic and electric connections can be made while the substructure 10 is in the lowered, transportation position prior to extending the hydraulic cylinders and prior to raising the substructure to the upstanding, in use position.
Whereas, the present invention has been described in relation to the drawings attached hereto, it should be understood that other and further modifications, apart from those shown or suggested herein, may be made within the spirit and scope of this invention. | A process to transport and assemble a drilling or workover rig substructure. The process includes the steps of transporting a driller side substructure section and an off driller side substructure section to a rig site so that the sections are spaced from and parallel to each other. A center substructure section is transported to the rig site. The center substructure section is moved into a space between the driller side and the off driller side sections. The center substructure section is thereafter connected to the driller side and to the off driller side subsections. A floor of the driller side substructure and a floor of the off driller side substructure are raised while both connected to the center substructure section from a transport position to a use position while maintaining the floors parallel to the bases. | 4 |
BACKGROUND OF THE INVENTION
This invention relates generally to air valves and more particularly to air valves designed to minimize icing and improve efficiency for a diaphragm pump or the like.
This invention relates to an improved fluid operated, double diaphragm pump, and, more particularly, to the pilot valve construction for such a pump.
The use of a double diaphragm pump to transfer materials is known. Typically such a pump comprises a pair of pumping chambers with a pressure chamber arranged in parallel with each pumping chamber in a housing. Each pressure chamber is separated from its associated pumping chamber by a flexible diaphragm. As one pressure chamber is pressurized, it forces the diaphragm to compress fluid in the associate pumping chamber. The fluid is thus forced from the pumping chamber. Simultaneously, the diaphragm associated with the second pumping chamber is flexed so as to draw fluid material into the second pumping chamber. The diaphragms are reciprocated in unison in order to alternately fill and evacuate the pumping chambers. In practice, the chambers are all aligned so that the diaphragms can reciprocate axially in unison. In this manner the diaphragms may also be mechanically interconnected to ensure uniform operation and performance by the double acting diaphragm pump.
Various controls have been proposed as the major distribution valve for providing a pressurized motive fluid, e.g., pressurized air, to the chambers associated with the double acting diaphragm pump. An exemplary control is shown in commonly assigned U.S. Pat. No. 4,854,832, in which a double diaphragm pump has a major distribution valve which includes a spool actuator that receives a sliding “D” valve. The spool actuator has a series of different diameters so as to provide for actuation is response to pressure differential thereby shifting the “D” valve between passageways to fill and exhaust the air chambers that drive the pump.
In designing air motor valving used to control the feed air to and exhaust air from the diaphragm chambers of such pumps, however, it is desirable to exhaust the diaphragm chambers as quickly as possible in order to obtain a fast switch over and high average output pressures. To achieve rapid exhaust times, larger distribution valves such as a elastomer-fitted or close fit spool-type valves are typically provided having larger porting that permits the rapid exhausting of air. Large temperature drops are generated with these larger valves, however, which cause the valve to become extremely cold and can cause ice formation from moisture in the exhaust air.
In order to minimize icing and improve the efficiency of the pump, commonly assigned U.S. Pat. No. 5,584,666, discloses a diaphragm pump having air valves designed to divert cold exhaust air from the major distribution valve. These air valves are bypass check valves, also known as “quick dump” valves, which are used in conjunction with spool valves due to their ability to pass large volumes of air in a relatively small package.
However, spool-type valves consist of many parts, which include rubber seals, or can be of the type which use close or lap fits to eliminate the elastomeric seals. Elastomer-fitted spools function well in dirty wet air and will not leak air when the pump stalled against backpressure. The elastomers used in an elastomer-fitted spool, however, are susceptible to chemical attack from airborne lubricants, which can cause the valve to hang up or stick. The lapped or close-fit spools eliminate parts but typically require constant lubrication to prevent sticking and do not function well with dirty air. Because there also must be some clearance between the spool and housing, air leakage will occur when the pump is stalled against backpressure, thus wasting compressed air.
The foregoing illustrates limitations known to exist in present devices and methods. Thus, it is apparent that it would be advantageous to provide an alternative directed to overcoming one or more of the limitations set forth above. Accordingly, a suitable alternative is provided including features more fully disclosed hereinafter.
SUMMARY OF THE INVENTION
In one aspect of the present invention this is accomplished by providing a reduced icing valve for a gas-driven motor and a reciprocating double diaphragm pump having a shiftable valve for alternatively supplying a motive gas through first and second supply ports to opposed first and second power pistons in opposed motive gas chambers, respectively, and for effecting alternating exhaust of the chambers. The shiftable valve is provided with an insert that deflects, away from the shiftable valve, air entering from each of the bypass valves until the bypass valves are fully actuated by the exhaust gas from the motive gas chambers. The shiftable valve is further provided with bypass valves independent of and intermediate the shiftable valve and each of the first and second motive gas chambers for bypassing the shiftable valve by exhaust gas from the motive gas chambers. The bypass valves are further actuated in an opposing direction by a supply source of motive gas to the chambers.
The foregoing and other aspects will become apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawing figures.
BRIEF DESCRIPTION OF THE DRAWING FIGURES
FIG. 1 is an elevational view of a diaphragm pump showing an air motor major valve according to the present invention and showing a housing chamber in partial section;
FIG. 2 is a cross sectional view taken along the section line “ 2 — 2 ” in FIG. 1, showing a reduced icing air valve according to the present invention having a major valve and bypass check valves;
FIG. 3 is a partial sectional, perspective view showing the reduced icing air valve according to the present invention;
FIG. 4 is a perspective view showing an adapter plate according to one aspect according to the present invention;
FIG. 5 is a top view of a center body housing of the diaphragm pump shown in FIG. 1; and
FIG. 6 is a top view of the adapter plate shown in FIG. 4 assembled to the top of the center body housing shown in FIG. 5 .
DETAILED DESCRIPTION OF THE INVENTION
According to the present invention, a reduced icing air valve is used having a major spool valve and valve plate combination to provide and exhaust motive air to and from an air motor. The present invention provides improvements to the diaphragm pumps and components shown and described in U.S. Pat. Nos. 4,854,832 and 5,584,666, the specifications of which are incorporated herein by reference.
According to a preferred embodiment of the present invention, an adapter plate is provided that permits the use of a “D” valve having a smaller valve insert than would otherwise be required while requiring fewer parts and the attendant difficulties provided by the typical spool valve constructions described above.
The drawings illustrate a typical double diaphragm pump incorporating the reduced icing air valve and major distribution valve construction of the present invention. Like numbers refer to like parts in each of the figures. Shown in FIG. 1 is a partial sectional view of a double diaphragm pump incorporating a main housing 100 that defines first and second opposed and axially spaced housing chambers. Each housing chamber includes a pressure chamber 26 and a fluid chamber 31 that are separated by a flexible diaphragm 29 as depicted by the partial sectional view of the left housing chamber in FIG. 1 . The pressure chamber, fluid chamber, and diaphragm in the right housing chamber are similarly arranged and form a mirror image of those components in the left housing chamber.
Each of the diaphragms 29 is fashioned from an elastomeric material as is known to those skilled in the art. The diaphragms 29 are connected mechanically by means of a shaft 30 that extends axially through the midpoint of each of the diaphragms. The shaft 30 is attached to the diaphragm 29 by means of opposed plates 33 on opposite sides thereof. Thus, the diaphragms 29 will move axially in unison as the pump operates by the alternate supply and exhaust of air to the pressure chambers of the pump as discussed in greater detail in the '832 and '666 patents. In brief, upon reciprocating the diaphragms of the pump, fluid that passes into each fluid chamber from-associated inlet-check valves is alternately compressed within and forced outwardly through associated outlet check valves. Operation of the fluid check valves controls movement of fluid in and out of the pump chambers causing them to function as a single acting pump. By connecting the two chambers through external manifolds, output flow from the pump becomes relatively constant.
The specific structure of the present invention relates to the construction of the reduced icing air valve and, more specifically, its major valve construction which provides and exhausts motive gas, respectively, to and from an air motor. Referring to FIG. 1, shown located between the left and right housing chambers is a center body housing 6 to which is attached to a valve block or body 2 having an air inlet 121 . As shown in FIG. 2, valve block 2 is generally a two piece construction that facilitates the assembly of a major valve that is comprised of the valve block 2 , a spool 1 , a valve insert 70 , a valve plate 3 , quick dump or bypass check valves 4 and 5 , and center body housing 6 .
Spool 1 is a differential piston having a large diameter end 170 and a small diameter end 160 as shown in FIG. 2 . Small diameter end 160 and large diameter end 170 include annular grooves having seals 164 and 174 which engage against the walls of a chamber 84 located in valve body 2 . Spool 1 also includes an annular groove 68 which receives a valve insert 70 that extends through the wall of valve body 2 and slides against valve plate 3 . The motion of valve insert 70 is limited by the wall of valve body 2 to correspond with the range of motion of the travel of the spool 1 in chamber 84 . The valve insert 70 is constructed so as to alternately connect an exhaust aperture 35 with a first aperture 34 and a second aperture 36 defined through the valve plate 3 . The spacing and position of valve insert 70 and the relative positions of exhaust aperture 35 , first aperture 34 , and second aperture 36 are such as to be consistent with the operation of the device as will be described below. Fluid pressure port 86 connects chamber 84 to provide air pressure from air inlet 121 to the pilot piston 7 during operation as described below which operates the double acting diaphragm pump.
Preferably, valve plate 3 and valve insert 70 are constructed of materials that are chemically inert and/or are internally lubricated to minimize chemical compatibility problems and reduce frictional loads, respectively, while also permitting the use of motive gas sources that are dirty.
Shown in FIG. 2 is an end view of a pilot valve consisting of a pilot piston 7 and an actuator pin 9 that extends into left pressure chamber 26 as shown in FIG. 1 . Not shown is a second actuator pin that is located in line with and on the opposite side of pilot piston 7 and extends into the right pressure chamber. During operation of the pump, as the diaphragms reciprocate the diaphragm plates alternately contact the actuating pins causing the pilot piston 7 to shift position. This shift in position of pilot piston 7 causes pneumatic pilot signals received from port 86 and through passage 186 to be sent to the front face 180 of spool 1 via a passage 190 and a port 90 and, alternately, to exhaust chamber via passage 200 . When a pilot signal is provided from port 86 to port 90 via pilot piston 7 , spool 1 shifts left. When a signal is not provided to port 90 , spool 1 shifts right due to supply air in chamber 84 acting on the back side of large diameter end 170 . In this manner, pilot piston 7 causes spool 1 to shift within valve body 2 at the end of each pump stroke thereby alternating the exhausting and filling of the pressure chambers and their corresponding fluid chambers. Preferably, pilot piston 7 is a differential piston having a large diameter end and a small diameter end such that air pressure acting on the large diameter of the piston will force the piston to one side when a pilot signal from chamber 84 is not provided to port 90 .
Quick-dump valves 4 and 5 are elastomeric check valves like those described in the '666 patent that sit in chambers 24 and 25 , respectively. As shown in FIGS. 1 and 2, chamber 24 is in fluid communication with left pressure chamber 26 via port 27 and vented via port 156 to an exhaust chamber 23 that exhausts to atmosphere via an exhaust port 123 . Chamber 25 is similarly vented to exhaust chamber 23 via port 155 and in fluid communication with right pressure chamber (not shown).
During operation of the pump, when spool 1 is in its extreme left position as shown in FIG. 2, supply air from inlet 121 passes through port 86 , pilot piston 7 , and passage 190 to port 90 . The front face 180 of spool 1 is thereby connected to the chamber 84 and thus to a pressurized source of fluid to maintain the spool I in the position shown in FIG. 1 . Simultaneously, because of the position of the valve insert 70 , supply air from inlet 121 flows from chamber 84 through the second aperture 36 in valve plate 3 and into chamber 24 . The air impinging on the upper surface of bypass check valve 4 forces it to seat and seal off exhaust port 156 . The air flow also deforms the lips of the elastomeric check such that air flows around the valve into port 27 and into left pressure chamber 26 . Thus, air pressure acting on the diaphragm 29 forces it to the left expelling fluid from the fluid chamber 31 through an outlet check valve. The shaft 30 likewise moves to the left as does the right diaphragm (not shown) which causes air to exhaust from the right pressure chamber. Pumped fluid is drawn into the right fluid chamber while fluid is pumped from the left fluid chamber 31 .
At the same time left pressure chamber 26 is filling, the air above valve 5 has been exhausted up through the first aperture 34 in valve plate 3 . Because valve insert 70 does not permit the air above the bypass check valve 5 to pass upward into valve body 2 , the exhaust aperture 35 in valve plate 3 is connected to exhaust chamber 23 by porting. In this manner, the air above the quick dump valves is directed by valve insert 70 back down through the exhaust aperture 35 in valve plate 3 and ported to exhaust which causes a pressure differential to occur between chambers 24 and 25 . The lips of valve 5 relax against the wall of chamber 25 . By this configuration, the combination of a valve insert 70 with quick dump, bypass check valves 4 , 5 is provided to permit the rapid exhaust of the pressure chambers through the quick dump valves and while using a minimum number of parts.
As air begins to flow from right pressure chamber upward through chamber 25 , it forces valve 5 to move upward to seat against valve plate 3 and seal off chamber 25 from the major valve while also opening port 155 . Exhaust air is dumped through port 155 into exhaust chamber 23 .
As the diaphragms move to the left, movement of the actuator pin located in the right pressure chamber is effected due to engagement of diaphragm plate located therein, thereby forcing the pilot piston to shift. Upon such transfer, the exhaust passages 190 and 200 are connected by the pilot piston and, thus, open to exhaust chamber 23 . In the absence of the pilot signal to port 90 , the supply air pressure within chamber 84 exerted on the backside of large diameter end 170 causes spool 1 , and valve insert 70 with it, to move right. Pressurized air then flows from air inlet 121 into chamber 25 causing the right pressure chamber to fill and the diaphragm located therein to move to the right. This in turn causes the connecting shaft 30 to move the left diaphragm 29 to the right, thereby exhausting the left pressure chamber 26 and causing the left fluid chamber 31 to fill.
The movement of plate 33 to the right in FIG. 1 will ultimately engage that plate with the actuator pin 9 , thereby causing the pilot piston 7 and, in turn, spool 1 back again effecting movement to the left of the diaphragms and shaft 30 . In this manner, the reversal of operation of the pump is effected, which will continue to oscillate or cycle as long as air is supplied through the inlet 121 .
While the '666 Patent discusses the incorporation of valves including “D” valves into diaphragm pumps having quick dump valves, the efficient interconnection of such valves in combination is most desirable. In incorporating a “D” valve into an air motor, the size of the valve insert is dictated by the span between the passages to be connected. The size of the valve insert used, in turn, determines the amount of friction encountered by the insert when moving against the valve plate. When using a larger valve insert to direct a motive gas into and out of a motor, a larger force is exerted by the gas on the valve insert due to the larger area presented by the valve insert. This increased force increases the frictional force of the valve insert against the valve plate and makes its movement more difficult during pump operation thereby decreasing the efficiency of the pump as more air is required to create the increased force required. Thus, the use of a smaller valve insert is preferred to decrease the frictional forces acting on the “D” valve and increase the efficiency of the pump. However, the span of the passages to be connected in a diaphragm pump generally calls for the use of a larger valve insert.
According to a preferred embodiment of the present invention, the porting between the exhaust aperture 35 of valve plate 3 and exhaust chamber 23 may be achieved through an adapter plate 50 , best seen in FIGS. 4 and 6, which minimizes the gap between the ports to be connected. Adapter plate 50 is shown in the sectional view of FIG. 3 disposed between valve plate 3 and bypass valves 4 , 5 . The adapter plate 50 comprises a first air path 54 and a second air path 56 that are in fluid communication with first aperture 34 and second aperture 36 , respectively. As shown in FIGS. 5 and. 6 , an exhaust vent 55 having two exhaust ports 51 is located between the first air path 54 and second air path 56 and connects exhaust aperture 35 to exhaust via exhaust apertures 52 located in center body housing 6 .
As shown in FIGS. 4 and 6, the exhaust vent 55 is, preferably, curvilinear-shaped and, most preferably, serpentine-shaped thereby minimizing the distance between said first and second air paths 54 , 56 . To provide air logic for shifting the shiftable valve, adapter plate 50 further comprises pilot signal paths 186 , 190 for connecting a pilot valve in fluid communication with the shiftable valve. Gaskets 60 , 61 , 62 , 63 , 64 , and 65 are provided as shown in FIGS. 5 and 6 to seal interconnecting air passages upon assembly of the center body housing 6 , adapter plate 50 , valve plate 3 , and valve body 2 .
There has been set forth a preferred embodiment of the invention. However, the invention may be altered or changed without departing from the spirit or scope thereof. The invention, therefore, is to be limited only by the following claims and their equivalents. | A reduced icing valve for an gas-driven motor and a reciprocating double diaphragm pump is provided having a shiftable valve for alternatively supplying a motive gas through first and second supply ports to opposed first and second power pistons in opposed motive gas chambers, respectively, and for effecting alternating exhaust of the chambers. The shiftable valve is provided with an insert that deflects, away from the shiftable valve, air entering from each of the bypass valves until the bypass valves are fully actuated by the exhaust gas from the motive gas chambers. The shiftable valve is further provided with bypass valves independent of and intermediate the shiftable valve and each of the first and second motive gas chambers for bypassing the shiftable valve by exhaust gas from the motive gas chambers. The bypass valves are further actuated in an opposing direction by a supply source of motive gas to the chambers. | 5 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a continuation application of U.S. patent application Ser. No. 12/233,483, filed Sep. 18, 2008, entitled LESS LETHAL AMMUNITION, which claims the benefit of priority to U.S. Provisional Patent Application Ser. No. 60/994,336 filed Sep. 18, 2007, entitled RING AIRFOIL GLIDER AMMUNITION LESS LETHAL, both of which are incorporated herein by reference.
FIELD OF THE INVENTION
The present invention pertains to ammunition, and in particular to less-lethal munitions incorporating sub-caliber projectiles.
SUMMARY OF THE INVENTION
One aspect of the present invention pertains to embodiments including a sabot for pushing a projectile such that the projectile exits the muzzle of the gun with the sabot being retained within the barrel.
Yet another aspect of the present invention pertains to a multi-piece sabot, in which a portion of the sabot pushes a projectile, and a portion of the sabot (either the same portion or a different portion) is ejected from the muzzle of the gun barrel.
Yet another aspect of some embodiments of the present invention pertain to methods and apparatus for linking together multiple munitions for semi-automatic or automatic firing of the munitions.
It will be appreciated that the various apparatus and methods described in this summary section, as well as elsewhere in this application, can be expressed as a large number of different combinations and subcombinations. All such useful, novel, and inventive combinations and subcombinations are contemplated herein, it being recognized that the explicit expression of each of these myriad combinations is excessive and unnecessary.
These and other aspects and features of various embodiments will be shown in the drawings, claims, and text that follows.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 a is a cross sectional elevated view of ammunition according to one embodiment of the present invention.
FIG. 1 b is an exploded cross sectional view of the ammunition of FIG. 1 a.
FIG. 2 illustrates a cross sectional view of the round of FIG. 1 a , feeding into chamber of a gun.
FIG. 3 illustrates a cross sectional view of the round of FIG. 1 a chambered at the firing point in a gun barrel.
FIG. 4 illustrates a cross sectional view of the round of FIG. 1 a as the round telescopes and fires the projectile.
FIG. 5 illustrates a cross sectional view of the round of FIG. 1 a as the projectile is launched in the barrel chamber.
FIG. 6 illustrates a cross sectional view of the round of FIG. 1 a as the projectile is released to travel down the gun bore and the round begins to eject.
FIG. 7 illustrates a cross sectional view of the assembled ammunition round as the projectile, and F.O.D. and sabot exits the muzzle.
FIG. 8 illustrates a cross sectional view of a ring airfoil projectile according to one embodiment of the present invention.
FIG. 9 illustrates an elevated cross sectional view of ammunition according to another embodiment of the present invention. FIG. 10 illustrates an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 10 is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 11 is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 12 is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 13 a is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 13 b is a cross sectional representation of the sabots of FIG. 13 a after separation.
FIG. 13 c is a perspective photographic representation of the linkage assembly for the round of FIG. 13 a.
FIG. 14 is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 15 is an elevated cross sectional view of a round according to another embodiment of the present invention.
FIG. 16 a is an elevated cross sectional view of a munition according to another embodiment of the present invention.
FIG. 16 b is a side perspective photographic view of the apparatus of FIG. 16 a , except without the linkage.
FIG. 16 c is a perspective photographic representation of a portion of the apparatus of FIG. 16 b.
FIG. 16 d is a perspective photographic representation of a portion of the apparatus of FIG. 16 b.
FIG. 16 e is a perspective photographic representation of a portion of the apparatus of FIG. 16 b.
FIG. 16 f is a perspective photographic representation of a portion of the apparatus of FIG. 16 b.
FIG. 16 g is a perspective photographic representation of a portion of the apparatus of FIG. 16 b , with the linkage mounted.
FIG. 16 h is a perspective photographic representation of a portion of the apparatus of FIG. 16 b , with the linkage mounted.
FIG. 17 illustrates a cross sectional view of the round of FIG. 16 a feeding into a chamber of a gun.
FIG. 18 illustrates a cross sectional view of the round of FIG. 16 a chambered at the firing point in a gun barrel.
FIG. 19 illustrates a cross sectional view of the round of FIG. 16 a as the round telescopes and fires the projectile.
FIG. 20 illustrates a cross sectional view of the round of FIG. 16 a as the projectile is launched in the barrel chamber and the sabot is stopped.
FIG. 21 illustrates a cross sectional view of the round of FIG. 16 a as the projectile and petals are released to travel down the gun bore and the round begins to eject.
FIG. 22 is a partial cross sectional view of the munition of FIG. 16 a being automatically loaded into a gun.
FIG. 23 is a partial cross sectional view of the munition of FIG. 16 a being automatically loaded into a gun.
FIG. 24 is a partial cross sectional view of the munition of FIG. 16 a being automatically loaded into a gun.
FIG. 25 is a partial cross sectional view of the munition of FIG. 16 a being automatically loaded into a gun.
FIG. 26 is a partial cross sectional view of the munition of FIG. 16 a being automatically loaded into a gun.
DESCRIPTION OF THE PREFERRED EMBODIMENT
For the purposes of promoting an understanding of the principles of the invention, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, such alterations and further modifications in the illustrated device, and such further applications of the principles of the invention as illustrated therein being contemplated as would normally occur to one skilled in the art to which the invention relates.
The use of an N-series prefix for an element number (NXX.XX) refers to an element that is the same as the non-prefixed element (XX.XX), except as shown and described thereafter. As an example, an element 1020 . 1 would be the same as element 20 . 1 , except for those different features of element 1020 . 1 shown and described. Further, common elements and common features of related elements are drawn in the same manner in different figures, and/or use the same symbology in different figures. As such, it is not necessary to describe the features of 1020 . 1 and 20 . 1 that are the same, since these common features are apparent to a person of ordinary skill in the related field of technology. Although various specific quantities (spatial dimensions, temperatures, pressures, times, force, resistance, current, voltage, concentrations, etc.) may be stated herein, such specific quantities are presented as examples only, and are not to be construed as limiting.
Incorporated herein by reference are U.S. patent application Ser. No. 12/045,647, filed Mar. 10, 2008; and Ser. No. 12/181,190, filed Jul. 28, 2008.
FIGS. 1 a and 1 b show cross-sectional and exploded views of a munition 20 according one embodiment of the present invention. Ammunition 20 includes a payload section 60 supported by a launch support assembly 40 . Further, a telescoping assembly 30 co-acts with launch assembly 40 to provide a breech block resetting capability for automatic weapons. Ammunition 20 can be fired from any type of gun, including the Mk 19 machine gun, the Mk M203 and Milkor single shot weapons, as well as 37 mm guns.
Telescoping assembly 30 includes a support member 32 that is slidingly received within a pocket of launch support member 42 . Telescoping support further includes a pocket 32 . 3 that receives within it an explosive assembly 34 . In one embodiment, explosive assembly 34 includes an initiator 34 . 1 in fluid communication via a passageway 34 . 3 within packing 34 . 2 to an explosive charge 34 . 4 . A resilient seal 36 provides sealing of the exploded charge 34 . 4 between members 32 and 34 prior to the rearward telescoping of member 32 relative to member 34 . Circumferential abutment 32 . 4 interacts with abutment 42 . 4 to limit the sliding of member 32 relative to member 42 . In some embodiments, telescoping assembly 30 further includes a ball-shaped firing pin 37 that is launched into and thereby causes ignition of initiator 44 . 1 during firing of ammunition 20 . Telescoping assembly 30 is preferably present in those versions of ammunition 20 that are fired from automatic weapons. Some embodiments of the present invention pertain to single shot weapons that do not need the function provided by telescoping assembly 30 .
Launch support assembly 40 provides secure mechanical coupling to the firing chamber of a gun, supports payload section 60 , slidingly couples to assembly 30 as previously described, and further supports a linkage assembly 24 . Linkage assembly 24 , as shown in FIGS. 1 a and 1 b , is a sliding link assembly that couples adjacent ammunitions 20 to each other. Linkage assembly includes a seal and retaining member 24 . 1 that is received on the outer diameter 42 . 11 of support 42 . A link mount 24 . 2 is slidingly received over the outer diameter of retainer 24 . 1 . A first Link 24 . 3 is tightly secured to the outer diameter of link mount 24 . 2 , and further receives and retains a captured coupling link 24 . 4 that couples to another coupling link of an adjacent ammunition 20 . Operation of the links, as well as operation of a munition, will be shown in FIGS. 29-34 that follow.
Support member 42 of Launch support assembly 40 further includes within it a pocket 42 . 3 that receives an explosive assembly 44 . Explosive assembly includes an initiator 44 . 1 that is in fluid communication with an explosive charge 44 . 4 by way of a central passage 44 . 3 within packing material 44 . 2 .
Explosive charge 44 . 4 is placed within a combustion chamber 42 . 1 of support 42 . A plurality of gas release passages 42 . 5 provide fluid communication of the combusted explosive charge with a plurality of hemispherical balls at the exit of the passage.
In some embodiments, one or both of the combustion chambers 32 . 1 or 42 . 1 can include a rupture diaphragm such as a copper disc that is conformally placed between the explosive charge and the chamber defined by corresponding member 32 or 42 . This disc contains the explosive gases until they reach sufficient pressure to rupture the disc wall and subsequently release the combusted gases into the corresponding gas passages 32 . 5 or 42 . 5 .
Extending from one end of support 42 is a rod 42 . 7 that includes a receptacle for a fastener, such as threaded receptacle 42 . 9 . Support 42 further includes a circumferentially extending shoulder 42 . 6 located proximate to the end of gas release passages 42 . 5 . A pocket is formed around the base of rod 42 . 7 between the outer diameter 42 . 8 of the rod and the inside of shoulder 42 . 6 .
A payload section 60 is received on rod 42 . 7 and shoulder 42 . 6 of support member 42 . Payload section 60 includes a sabot that is fittingly received on shoulder 42 . 6 . A frangible retainer 64 is received on the distal end of rod 42 . 7 . A ringed airfoil projectile 80 is captured between sabot 62 and retainer 64 .
Sabot 62 includes a curving annular middle section located between an inner cylindrical portion 62 . 2 and an outer cylindrical portion 62 . 1 . The inner face of the annular midsection is received against shoulder 42 . 6 . The inner diameter of cylindrical section 62 . 2 is in sliding contact with outer diameter 42 . 8 of rod 42 . 7 . The outer diameter of outer cylindrical portion 62 . 1 includes an outer most diameter that is in sliding contact with the inner diameter and rifling 22 . 2 of the barrel 22 . 1 of a gun 22 , as will be shown and described for FIGS. 29-34 . Sabot 62 further includes a plurality of circumferentially extending drive features 62 . 4 that couple to corresponding and complementary driven features of ring airfoil 80 .
Retainer 64 includes a center support ring 64 . 2 that is held on the end of rod 42 . 7 by a fastener or other coupling means 46 . A plurality of outwardly extending and separated petals 64 . 1 extend from support ring 64 . 2 a frangible feature such as a notch is preferably located at the connection of a petal to the support ring, and acts as a stress riser during operation. Each petal extends outwardly and aft (aft being defined as the direction toward telescoping assembly 30 and forward being defined as the direction toward payload section 60 and further toward the open end of the gun barrel), and on the aft face of each petal there is a small pocket for receiving within it the leading edge 90 of ring air foil 80 . Ring air foil 80 is captured on ammunition 20 between sabot 62 and retainer 64 .
FIG. 8 shows cross sectional, side elevational view of ring airfoil 80 . Airfoil 80 comprises a substantially hollow, annular ring wall. The wall of airfoil 80 has an airfoil section 94 that includes a cambered outer surface 82 and cambered inner surface 84 . These inner and outer surfaces 82 and 84 , respectively, meet at a substantially blunt leading edge 90 , and at a substantially tapered trailing edge 92 . The inner surface 84 of airfoil 80 defines a substantially open central aperture 86 . Preferably, ring airfoil 80 is a body of revolution formed by rotating airfoil section 94 about central axis 86 . 1 . Ring airfoil 80 has a length 86 . 2 from leading edge 90 to trailing edge 92 , and an outer diameter 82 . 1 extending across the outermost portion of outer surface 82 , and an innermost diameter or throat 86 . 4 extending across the innermost portion of inner surface 84 . In some embodiments, trailing edge 92 includes a plurality of drive features (such as rectangular cutouts) that mate with complementary features on sabot 62 .
Tables 1 and 2 present data for outer diameter and inner diameter, respectively, related to a programming table of values for a computer numerically controlled machine to fabricate a projectile according to one embodiment of the present invention. In both of these tables, the first column represents the diametrical distance (or twice the radius from the center line), and the second column represents a location along the Z Axis. A representative projectile can be machined from this data. If a cutting tool having a radius of about 0.016 is positioned in accordance with this data, it will have a tangent point of contact on the airfoil surface. In one embodiment, the overall length of the projectile is about 1 inch.
TABLE 1
Diametral Distance
Axial Location
1.4364
+.0158
1.4422
+.0153
1.4476
+.0148
1.4530
+.0140
1.4586
+.0131
1.4644
+.0119
1.4708
+.0104
1.4774
+.0088
1.4842
+.0066
1.4908
+.0045
1.4968
+.0022
1.5032
−.0004
1.5086
−.0029
1.5136
−.0055
1.5188
−.0064
1.5236
−.0113
1.5280
−.0145
1.5324
−.0179
1.5366
−.0215
1.5410
−.0255
1.5452
−.0298
1.5492
−.0344
1.5532
−.0393
1.5572
−.0445
1.5812
−.0502
1.5850
−.0582
1.5888
−.0627
1.5726
−.0697
1.5762
−.0771
1.5798
−.0850
1.5834
−.0934
1.5868
−.1024
1.5902
−.1125
1.5936
−.1230
1.5968
−.1340
1.5996
−.1457
1.6028
−.1582
1.6056
−.1713
1.6064
−.1755
1.6090
−.1898
1.6116
−.2048
1.6138
−.2207
1.6180
−.2375
1.6176
−.2519
1.6194
−.2705
1.6210
−.2901
1.6222
−.3109
1.6234
−.3329
1.6238
−.3420
1.6246
−.3888
1.6252
−.3907
1.6252
−.4127
1.6252
−.4346
1.6246
−.4523
1.6240
−.4888
1.6228
−.4854
1.6218
−.4987
1.6200
−.5181
1.6178
−.5373
1.6156
−.5558
1.6134
−.5715
1.6108
−.5886
1.6076
−.6057
1.6042
−.6229
1.5998
−.6434
1.5956
−.6612
1.5912
−.6789
1.5912
−.6789
1.5864
−.6985
1.5812
−.7143
1.5758
−.7315
1.5704
−.7484
1.5644
−.7652
1.5574
−.7843
1.5508
−.8010
1.5440
−.8180
1.5366
−.8363
1.5288
−.8532
1.5210
−.8694
1.5138
−.8847
1.5080
−.8995
1.4982
−.9143
1.4944
−.9213
1.4882
−.9362
1.4782
−.9534
1.4648
−.9724
1.4554
−.9881
1.4463
−.1.0028
(off surface for reference of
shape only +1 −.0 )
1.4394
−.1.10136
(off surface for reference of
shape only)
TABLE 2
Diametral Distance
Axial Location
1.4284
+.0158
1.4148
+.0146
1.3994
+.0125
1.3842
+.0091
1.3710
+.0051
1.3688
+.0002
1.3470
−.0054
1.3416
−.0083
1.3294
−.0157
1.3156
−.0253
1.3054
−.0332
1.2932
−.0437
1.2878
−.0492
1.2708
−.0868
1.2544
−.0859
1.2392
−.1054
1.2282
−.1254
1.2142
−.1458
1.2036
−.1668
1.1946
−.1878
1.1888
−.2100
1.1808
−.2323
1.1754
−.2544
1.1710
−.2780
1.1672
−.2971
1.1640
−.3178
1.1616
−.3381
1.1588
−.3771
1.1584
−.3961
1.1588
−.4155
1.1602
−.4382
1.1622
−.4583
1.1650
−.4817
1.1688
−.5085
1.1734
−.5326
1.1788
−.5601
1.1848
−.5890
1.1918
−.6182
1.1994
−.6468
1.2076
−.6747
1.2182
−.7020
1.2258
−.7285
1.2358
−.7544
1.2464
−.7796
1.2578
−.8041
1.2698
−.8284
1.2828
−.8885
1.2988
−.8776
1.3118
−.9025
1.3278
−.9277
1.3446
−.9530
1.3824
−.9788
1.3812
Tables 3 and 4 present data for outer diameter and inner diameter, respectively, related to a programming table of values for a computer numerically controlled machine to fabricate a projectile according to another embodiment of the present invention. In both of these tables, the first column represents the diametrical distance (or twice the radius from the center line), and the second column represents a location along the Z Axis. A representative projectile can be machined from this data. If a cutting tool having a radius of about 0.016 is positioned in accordance with this data, it will have a tangent point of contact on the airfoil surface. In one embodiment, the overall length of the projectile is about 1 inch.
TABLE 3
Diametral Distance
Axial Location
1.4364
+.0156
1.4422
+.0153
1.4476
+.0148
1.4530
+.0140
1.4586
+0131
1.466
+0.119
1.4708
+.0104
1.4774
+.0086
1.4842
+.0066
1.4908
+.0045
1.4968
+.0022
1.5032
−.0004
1.5086
−.0029
1.5138
−.0055
1.5188
−.0084
1.5236
−.0113
1.5280
−.0145
1.5324
−.0179
1.5366
−.0215
1.5410
−0.255
1.5452
−.0298
1.5492
−.0344
1.5532
−.0393
1.5572
−.0445
1.5612
−.0502
1.5650
−.0682
1.5688
−.0627
1.5726
−.0697
1.5762
−.0771
1.5798
−.0850
1.5834
−.0934
1.5868
−.1024
1.5902
−.1125
1.5936
−.1230
1.5968
−.1340
1.5998
−.1457
1.6028
−.1582
1.6056
−.1713
1.6064
−.1755
1.6090
−.1898
1.6116
−.2048
1.6138
−.2207
1.6160
−.2375
1.6176
−.2519
1.6194
−.2705
1.6210
−.2901
1.6222
−.3109
1.6234
−.3329
1.6238
−.3420
1.6246
−.3666
1.6252
−.3907
1.6252
−.4127
1.6252
−.4346
1.6246
−.4523
1.6240
−.4888
1.6228
−.4854
1.6218
−.4987
1.6200
−.5181
1.6178
−.5373
1.6156
−.5556
1.6134
−.5715
1.6106
−.5886
1.6076
−.6057
1.6042
−.6229
1.5998
−.6434
1.5956
−.6612
1.5912
−.6789
1.5864
−.6965
1.5812
−.7143
1.5758
−.7315
1.5704
−.7484
1.5644
−.7652
1.5574
−.7843
1.5508
−.8010
1.5440
−.8180
1.5366
−.8353
1.5286
−.8532
1.5210
−.8694
1.5136
−.8847
1.5060
−.8995
1.4982
−.9143
1.4944
−.9213
1.4862
−.9362
1.4762
−.9534
1.4648
−.9724
1.4554
−.9881
1.4463
−.1.0028
1.4394
−.1.0136
TABLE 4
Diametral Distance
Axial Location
1.3918
+.0156
1.3782
+.0146
1.3628
+.0125
1.3476
+.0091
1.3344
+.0051
1.3220
+.0002
1.3104
−.0054
1.3050
−.0083
1.2928
−.0157
1.2790
−.0253
1.2688
−.0332
1.2566
−.0437
1.2510
−.0492
1.2340
−.0668
1.2178
−.0859
1.2026
−.1054
1.1896
−.1254
1.1776
−.1458
1.1580
−.1878
1.1502
−.2100
1.1440
−.2323
1.1388
−.2544
1.1344
−.2760
1.1306
−2971
1.1274
−.3178
1.1250
−.3381
1.1222
−.3771
1.1218
−.3961
1.1222
−.4155
1.1236
−.4362
1.1256
−.4583
1.1284
−.4817
1.1322
−.5065
1.1368
−.5326
1.1422
−.5601
1.1482
−.5890
1.1552
−.6182
1.1628
−.6468
1.1710
−.6747
1.1796
−.7020
1.1890
−.7285
1.1990
−.7544
1.2098
−.7796
1.2210
−.8041
1.2330
−.8284
1.2462
−.8685
1.2602
−.8776
1.2752
−.9025
1.2910
−.9277
1.3080
−.9530
1.3258
−.9786
1.3446
−1.007
The following is a description of the firing of ammunition as shown in FIGS. 2-7 .
Upon being on the bolt face in the ready battery position, latched and ready to be fired, the trigger is pulled.
The bolt travels forward until the firing pin 22 . 4 is released, about 1″ from the breech face 22 . 3 .
The pin strikes the aft telescoping charges primer initiating the propellant; simultaneously an initiation ball 37 is propelled forward to a primer 34 . 1 for the forward payload propelling charge, and the expanding gas reacts against the telescoping piston to open the action and auto load function the gun.
The forward payload propelling charge expands against the sabot/pusher 62 pushing it forward while fracturing the projectile retainer 64 along one or more separation groove(s) on the central hub of the retainer releasing the sabot and projectile assembly for forward travel.
The sealing and rotating outer diameter 62 . 1 of sabot 62 seals the propelling gas from the action at the forcing cone of the chamber. The sabot/projectile assembly 160 is pushed along the bore and along the center guide mandrill 42 . 7 , throughout the launch sequence.
The sabot/projectile assembly travels down the bore to the end of the guide mandrill having spin imparted to the assembly by the action of rifling 22 . 2 in the gun bore 22 . 1 rotating the sabot 62 which transfers the rotation by the action of drive dogs 62 . 4 on its forward face engaging slots 88 in the tail 92 of the ring airfoil projectile 80 .
As the sabot leaves the mandrill the propelling gas are vented down the center of the sabot down the bore ahead of the sabot/projectile assembly, protecting the ring airfoil projectile from disturbance by the gas, at which point the maximum velocity is achieved for both the sabot and projectile.
The sabot immediately begins to decelerate due to friction with the bore. This causes the projectile to separate, as it has little or no contact with the bore and little friction retarding its passage down the bore.
The projectile rides a turbulent boundary layer of air between its outer diameter and the bore guiding and centering it until it exits the muzzle. The sabot exits the muzzle at greatly reduced energy. The ring airfoil 80 is free to fly towards the target.
As the ring airfoil 80 travels through the air, if it is thought that a higher pressure is created in the duct 86 through it by the comparatively more cambered shaped of the airfoil surface on the inside of the duct in contrast to the lesser curved shape on the periphery of the ring airfoil creating a lower static pressure on the ring airfoil outer surface 82 . This increased drag helps stabilize the projectile along with the gyroscopic spin imparted to it by action of the rifling, allowing the projectile to be less prone to curved flight paths and external disruptions such as cross wind and air disturbances. The center of pressure along the projectile longitudinal axis is aft or coincides with the center of mass. The action of the increased drag in the duct creates an aerodynamic stabilizing force on the projectile as if it has a tail much like an arrow, reducing the dependence on spin stabilization.
FIG. 9 illustrates a cross sectional view of an assembled ammunition round 120 having a forward hook for retaining the link mount 124 on the mandrill body 142 which is held in place on a shear shoulder 149 . 1 on a chamber seal 149 . Round 120 includes a chamber seal 149 that is attached to support member 142 . Preferably, seal 149 is fabricated from a plastic (such as ABS or aluminum) and is attached to body 142 with an interference fit. Chamber seal 149 includes an outwardly projecting sealing surface that forms a seal with the inner diameter barrel 22 . 1 so as to substantially obstruct the leakage of gas provided by gas release passages 142 . 5 .
In some embodiments, munition 120 includes a crimped opening 148 . 2 that serves to frictionally couple together supports 132 and 142 . Preferably, there are a plurality of discrete inward crimps 148 . 2 around the periphery of the aft end of body 142 . These crimps capture support 142 within the large inner pocket of member 142 , and prevent inadvertent telescoping of member 132 relative to member 142 during handling.
During firing, shoulder 149 . 1 of seal 149 is shorn when the bolt comes forward, forcing the link mount shoulder against the chamfer on the barrel breech. The shoulder on the link mount is milled flat to create clearance in the feed tray of the machine gun to prevent rubbing of the shoulder on the feed guide slots.
FIG. 10 illustrates a cross sectional view of an assembled ammunition round 220 in accordance with another embodiment. Round 220 includes a launch support assembly 240 that is threadingly engaged along interface 241 . 8 to a base 248 . Assembly 240 includes a support 242 that includes at least a portion of a combustion chamber 242 . 1 . Chamber 242 . 1 is generally shaped conically inward, and includes a plurality of gas passageways 242 . 5 that extend outwardly and into fluid communication with the underside of sabot 262 .
In some embodiments, launch assembly 240 is fabricated, assembled, shipped, and stored as a subassembly. During final assembly of round 220 , an explosive charge 244 is placed in combustion chamber 242 . 1 . A mating base 248 is prepared as a subassembly including a chamber seal 249 , primer holding 244 . 2 , and primer 244 . 1 . Subassemblies 240 and 248 are threadingly engaged to form a finished munition 220 .
Round 220 is adapted and configured for use in standard single shot launchers like the M203. The forward mandrill 242 can be affixed with a fixed cartridge rim 248 used in place of the telescoping components. Threaded interface 248 . 1 includes male and female threads that can be reversed on the components to be attached if desired.
The embodiment shown in FIG. 11 illustrates a cross sectional view of an assembled ammunition round 320 as another embodiment, Round 320 includes a launch support assembly 340 that is substantially the same as assembly 240 . However, round 320 includes a base assembly 348 adapted and configured for use in semi-automatic and automatic guns. Base 348 includes male threads for threadably coupling to the female threads of assembly 340 at threaded interface 348 . 1 .
Base 348 , when fully assembled, further includes a chamber seal 349 and packing 344 . 2 located within a central pocket. The assembled base 348 further includes an initiator 344 . 1 that provides ignition through central passage 344 . 3 to explosive charge 344 . 4 after being impacted by ball 337 . Ball 337 is retained within a pocket of support assembly 332 . A cover plate 350 is adhered to a face of support 332 to retain ball 337 in its pocket. In one embodiment, cover plate 350 comprises an aluminum diaphragm of about 0.006 inches thickness.
FIG. 11 includes a linkage assembly 324 and linkage interfaces that are different than those described for round 20 . Referring to FIG. 11 , and also to FIGS. 13 c , 16 a , 16 b , 16 g , and 16 h , which have related linkage features, body (or base) 348 includes a region 326 . 1 of reduced outer diameter immediately in front of a region 326 of increased outer diameter. Behind ridge 326 is an area 326 . 2 of constant diameter that is preferably about midway between diameters 326 . 1 and 326 . Preferably, diameter 326 . 2 is about the same as diameter 342 . 15 of support 342 .
Linkage assembly 324 is preferably spring loaded in tension around outer diameter 342 . 15 of body 342 . The spring tension of link 324 is chosen to securely locate linkage 324 on body 342 during pre-firing handling. In one embodiment, linkage 324 comprises two sheet metal stampings that overlap at the top and bottom (as shown in FIG. 11 ), and further which are spot welded together in the overlapping area 324 . 9 .
During firing, the movement by the breech block 22 . 3 of the gun 22 places round 320 into the firing chamber. Contact between the end of barrel 22 . 1 and the front face of linkage 324 forces link 324 to slide aft toward depression 326 . 1 . Since linkage 324 is placed in tension, this movement into an area of reduced diameter (relative to diameter 342 . 15 ) momentarily reduces the amount of tension. As the coaction of the end of the barrel and linkage 324 continues, link 324 is forced to pivot open toward the rear, and climb over ridge 326 . Preferably, the aft face of depression 326 . 1 and the forward face of ridge 326 are sloped to minimize gouging. As the backward action of link 324 continues, it climbs over ridge 326 and relocates on diameter 326 . 2 .
Regions of body 348 that contact linkage 324 are generally cylindrical and can include one or more milled flats to provide adequate clearance to parts of the gun and ammunition feed tray. Further, although generally cylindrical regions are shown and described, various embodiments of the present invention contemplate other types of surface features (including a plurality of circumferentially-space projections) that support the underside of linkage 324 as described herein as linkage 324 slides aftward over body 348 .
Round 320 includes a separate telescoping chamber (or base) 348 and mandrill body 332 to allow interchangeability with single shot rounds. The telescoping components needed for autoloading in a machine gun are separate from ring airfoil components. The buttress shoulder on the body of the round which is used to react against the barrel breech chamfer is milled flat to clear the feed tray of the gun and provide free clearance to the link as it is slide back by action of the bolt.
The embodiment shown in FIG. 12 illustrates a cross sectional view of an assembled ammunition round 420 as another embodiment. Round 420 includes means 464 . 4 for stopping sabot 462 . As shown in FIG. 12 , stopping means 464 . 4 includes an oversize washer mounted inbetween support ring 464 . 2 of retainer 464 and rod 442 . 7 of support member 442 . During firing of munition 420 , sabot 462 is pushed forward by combustion gases and is guided by both the inner diameter of barrel 22 . 1 and the outer diameter 442 . 8 of rod 442 . 7 . This guided, forward travel of sabot 462 pushes projectile 480 into the frangible retaining petals of retainer 464 . These petals break, and sabot 462 continues pushing projectile 480 toward the exit of the barrel. The sliding motion of sabot 462 stops when its forward face contacts the aft face of sabot stop 464 . 4 . After contact is made, projectile 480 continues forward and is ejected from the gun barrel. Sabot 462 is retained on rod 442 . 7 . Sabot stop 464 . 4 stops the sabot 462 from exiting the muzzle, and prevents the sabot from being a secondary projectile for both unwanted target impacts and to prevent distraction of the gunner's sighting ability by the sabot.
FIGS. 13 a , 13 b , and 13 c illustrate views of an assembled ammunition round 520 . Round 520 is the same as round 420 , except that a separate sabot stop 464 . 4 is replaced with a stop 564 . 4 that is molded integrally with retainer 564 .
Yet another feature of round 520 is the incorporation of a two piece sabot. A first, outer sabot 562 includes an outer diameter 562 . 1 that is in sealing contact with the inner diameter of the gun barrel to discourage leakage of combustion gas. Further, outer diameter 562 . 1 engages the rifling of the barrel and thereby impart spin to outer sabot 562 . Outer sabot 562 includes a plurality of driving features (dogs) 562 . 4 that engage the trailing end of projectile 580 , to thereby also imparts spin to projectile 580 . Yet other embodiments contemplate that either the inner sabot or outer sabot can include the drive dogs that engage the trailing edge of the projectile.
As best seen in FIG. 13 b , round 520 further includes an inner sabot 563 having an inner diameter 563 . 3 that is guided along the outer diameter of rod 542 . 7 . The outermost diameter of inner sabot 563 is adapted and configured with driving and sealing features 563 . 6 that interlock with corresponding features 562 . 6 of inner sabot 562 . As indicated by arrows 562 . 7 , the driving features preferably include contacting surfaces adapted and configured to transmit a force that has at least one vector component parallel to the axis of the gun barrel for transmitting propulsive load to the projectile. However, yet other embodiments of the present invention contemplate means for driving that include frictional, interference-type fits between the inner and outer sabots.
FIG. 13 c depicts one embodiment of the linkage assembly 524 of munition 520 . Linkage assembly 524 includes a first formed, sheet metal link 524 . 5 coupled to a second, formed, sheet metal link 524 . 6 by a plurality of spotwelds along upper and lower linkage overlapping portions 524 . 9 . Link assembly 524 further includes a T-pin 524 . 7 that is captured on a lateral side of link 524 . 5 . T-pin 524 . 7 is adapted and configured to couple within the slot 524 . 8 of linkage piece 524 . 6 . T-pin 524 . 7 and slot 524 . 8 are examples of complementary-shaped features for coupling to adjacent munitions in a linked belt.
FIG. 14 illustrates a cross sectional view of the assembled ammunition round 620 , another embodiment of the present invention. Round 620 includes a retainer 664 including a central rod 664 . 6 that threadably couples to threads 646 of support 642 . In one embodiment, retainer 664 further includes a sabot stop 664 . 4 for stopping the forward motion of sabot 662 . In some embodiments, the inner diameter 662 . 2 of sabot 662 is guided by the substantially aligned and parallel outer diameters of rod 642 . 7 and rod 664 . 6 . The present invention contemplates the fastening of a retainer 664 to a support 642 in which either component has male threads, and the other component has female threads. Further, other embodiments contemplate alternate means of fastening retainer 664 to support 642 , including the use of adhesives, and further the use of one-way interlocking features, such as the ratchet and lock features of some types of rivets. In the latter case, retainer 664 would be pressed onto rod 642 . 7 in a non-releasable manner.
FIG. 15 illustrates a cross sectional view of an assembled ammunition round 720 as another embodiment. Round 720 includes a threaded interface 748 . 1 between body 742 and outer support assembly (base) 748 in which support member 742 includes the male interface and base 748 includes the female interface. Yet other embodiments contemplate other means for coupling body 742 to base 748 , including the use of adhesives, and further the use of a one-way interlocking interface such as an internal ratchet and lock of a rivet. Other coupling ideas include an interference fit between body 742 and 748 .
FIGS. 16 a , 16 b , 16 c , 16 d , 16 e , 16 f , 16 g , and 16 h depict an ammunition round 820 according to another embodiment of the present invention. Round 820 includes a base 848 having a central projection 848 . 13 that is accepted within a compartment (or pocket) 842 . 13 within support body 842 . Projection 848 . 13 further includes a central passage 844 . 3 for communicating an ignition pulse from the primer to the explosive charge 844 . 4 . In one embodiment an o-ring seal 842 . 14 resides within a groove of pocket 842 . 13 for sealing of combustion gases. Base 848 includes female threads 848 . 6 that interface with male threads on base 842 (this thread orientation being interchangeable).
FIG. 16 d shows a launch support assembly 840 according to one embodiment of the present invention. Assembly 840 is a subassembly that is interchangeable on either single shot or automatic loading bases 848 . In one embodiment, munition 840 includes a retainer 864 , sabot 862 , projectile 880 captured between the retainer and sabot, and a base 842 that supports the retainer and sabot. Subassembly 840 can be coupled to a base by coupling means including threads, bayonet-type connections (such as those used with electrical connectors), adhesives, an interference fit, and/or shear pins (such as cold-rolled pins inserted through the walls.
The assembled base 848 further includes a telescoping support body 832 which is useful in reloading applications. Body 832 includes a chamber (or pocket) 832 . 13 that accepts within it a concave combustion chamber support 833 . Support 833 further includes within it an internal pocket that accepts a central projection 832 . 15 of body 832 . An o-ring seal 832 . 14 is located within a groove of either projection 832 . 15 or the corresponding pocket of support 833 for sealing of combustion gases.
Combustion chamber support 833 preferably defines at least a portion of a combustion chamber to house an explosive charge 834 . 4 . A plurality of gas passageways 832 . 5 extend outwardly from the combustion chamber (as best seen in FIG. 16 f ). In some embodiments, combustion chamber support 833 is an interference fit and is pressed into pocket 832 . 13 .
In one embodiment, retainer 864 is fabricated from high density polyethylene (HDPE). Projectile 880 is preferably fabricated from Noryl®. Body 842 , sabot 862 , and combustion chamber support 833 are preferably fabricated from a polymer such as ABS. Base body 848 is fabricated from an aluminum alloy such as 7075-T6. Support body 832 is preferably fabricated from aluminum such as 6020-T8.
FIGS. 17-21 show schematically the firing of a round 820 within a gun barrel 22 . 1 . The following is a description of the firing of ammunition as shown in FIGS. 17-21 . Upon being on the bolt face in the ready battery position, latched and ready to be fired, the trigger is pulled. The bolt travels forward until the firing pin 22 . 4 is released, about 1″ from the breech face 22 . 3 .
Referring to FIG. 18 , the pin strikes the aft telescoping charges primer initiating the propellant; simultaneously an initiation ball 837 is propelled forward to a primer 834 . 1 for the forward payload propelling charge, and the expanding gas reacts against the telescoping piston to open the action and auto load function the gun.
The forward payload propelling charge expands against the sabot/pusher 862 pushing it forward while fracturing the projectile retainer 864 along one or more separation groove(s) on the central hub of the retainer releasing the sabot and projectile assembly for forward travel.
Referring to FIG. 19 the sealing and rotating outer diameter 862 . 1 of sabot 862 seals the propelling gas from the action at the forcing cone of the chamber. The sabot/projectile assembly 160 is pushed along the bore and along the center guide mandrill 842 . 7 , throughout the launch sequence.
The sabot/projectile assembly travels down the bore to the end of the guide mandrill having spin imparted to the assembly by the action of rifling 22 . 2 in the gun bore 22 . 1 rotating the sabot 862 , which transfers the rotation by the action of drive dogs 862 . 4 on its forward face engaging slots 888 in the tail 892 of the ring airfoil projectile 880 .
Referring to FIG. 20 , the front surface of sabot 862 has contacted the aft facing surface of sabot stop 864 . 4 . Sabot 862 is unable to move past stop 864 . 4 , and comes to rest on rod 842 . 7 . However, projectile 880 is not stopped, and continues to fly within barrel 22 . 1 . In those embodiments having a two-piece sabot assembly, one sabot portion is stopped and retained on rod 842 . 7 , and the other portion continues its flight down the barrel, behind projectile 880 .
The projectile rides a turbulent boundary layer of air between its outer diameter and the bore guiding and centering it until it exits the muzzle. The sabot exits the muzzle at greatly reduced energy. The ring airfoil 80 is free to fly towards the target. The automatic loading features of gun 22 remove the fired round 820 from barrel 22 . 1 . Sabot 862 , since it is retained on member 842 , exists with the spent munition.
FIGS. 22-26 depict the co-action of spring-loaded link assembly 824 with barrel 22 . 1 during the automatic loading process. As round 820 is brought to the breech of barrel 22 . 1 , the overlapping portions 824 . 9 of link assembly 824 come into contact with and abut against the end 22 . 5 of barrel 22 . 1 (as best seen in FIG. 22 ). Continued motion of round 820 into barrel 221 causes link 824 to be held in position against barrel end 22 . 5 . As support assembly 848 continue to move into barrel 22 . 1 , the aft most edge of link assembly 824 moves into the region 826 . 1 of reduced diameter, such that link assembly 824 momentarily takes on a conical shape with reduced tension (as best seen in FIG. 23 ).
FIG. 24 shows that subsequent motion of round 820 into barrel 22 . 1 continues to move link assembly 824 in sliding motion over shoulder 826 of body 848 . Link assembly 824 thereby takes on a conical shape and increased tension, except in a direction different than that as shown in FIG. 23 . Referring to FIG. 25 , the continued motion of round 820 is stopped by the abutment of the forward edge of ridge 826 against chamfer 22 . 6 of barrel 22 . 1 .
In some embodiments, linkage assembly 824 is supported in a conical shape by both shoulder 826 and further by the diameter 826 . 2 of body 848 immediately aft of shoulder 826 . As shown in FIG. 26 , linkage 824 continues to slide along the curving and diametrically-reducing aft surface of should 826 , and linkage assembly 824 comes to rest on the aft portion of ridge 826 and on the diameter 826 . 2 of body 848 aft of the ridge.
The following figures are scaled drawings: 9 , 10 , 11 , 12 , 13 a , 14 , 15 , and 16 a . All of the munitions shown and described herein are applicable to guns ranging from about 36 mm to about 43 mm. In one embodiment, projectiles 80 weigh about 12 to 14 grams, and are launched with a muzzle exit velocity of about 100 mps. However, the invention is not so limited, and these dimensions and scalings are illustrative examples only.
Although what are shown and described are a variety of munitions including a ring airfoil projectile, the invention is not so limited, and contemplates the use and launching of any kind of projectile, including as non-limiting examples rubber bullets, bean bags, nets, balls, gas canisters, and also including lethal projectiles, and the like.
While the inventions have been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character, it being understood that only the preferred embodiment has been shown and described and that all changes and modifications that come within the spirit of the invention are desired to be protected. | In one embodiment, a less lethal munition including a ring airfoil projectile. The flight trajectory of the projectile has increased accuracy resulting from the aerodynamic stabilization of the projectile. In some embodiments, the projectile is both aerodynamically stabilized and spin stabilized. | 5 |
TECHNICAL FIELD OF THE INVENTION
This invention relates to Discrete MultiTone (DMT) and Orthogonal Frequency Division Multiplex (OFDM) systems and more particularly to a DMT/OFDM transceiver.
BACKGROUND OF THE INVENTION
In DMT/OFDM systems, bits in a transmit data stream are divided up into symbols which are then grouped and used to modulate a number of carriers. Each carrier is modulated using either Quadrature Amplitude Modulation (QAM), or Quadrature Phase Shift Keying (QPSK) and, dependent upon the characteristics of the carrier's channel, the number of source bits allocated to each carrier will vary from carrier to carrier. In the transmit mode, inverse Fast Fourier Transforms (iFFT's) are used to convert QAM modulated pairs into symbols for the transmitted signal. In the receive direction, Fast Fourier Transforms (FFT's) are used before QAM demodulation.
In typical systems, the discrete Fourier transform (DFT) or inverse discrete Fourier transform (iDFT) is performed using the Fast Fourier transform (FFT) operation. The FFT has the advantage that the number of operations compared to the DFT is significantly reduced. A “N” point DFT requires N^2 operations whilst an “N” point FFT requires N log 2 (N)/2 operations, a considerable saving.
As has already been noted the transmitter requires an inverse FFT while the receiver requires an FFT. In DMT systems, such as ADSL, these operations are typically performed by separate hardware or software modules or a single, double speed module used alternately for receive and transmit. An object of the present invention is how to make this less complex by using a single normal speed module, in hardware or software, to implement both functions, since this will result in a considerable reduction in computational complexity, besides less expense for silicon.
It is known from an article “ADSL, VDSL and Multicarrier Modulation” by John A. C. Bingham (John Wiley & Sons), that if the data for a FFT is only real valued, by packing odd and even samples into a complex array of half the original length, the FFT size may be reduced to half. The resultant, complex data output is separated by:
(1) Pre-processing the data such that when an iFFT is performed the real par contains even time samples and the imaginary part odd time samples:
Y[i]={X ( i )+ X *( N−i )]+ j[X ( i )− X *( N−i ) W^ ( N−i )}*
(where N is the size of the transform, e.g. a 256 point complex vector and X* is the complex conjugate). (2) Providing an input to the FFT which is a 256 point complex vector formed from the real 2N point data: the real part containing even sample points and the imaginary part odd sample points and post processing the FFT output:
Y[i ]=0.5 [X ( i )+ X *( N−i )]− j/ 2 [X ( i )− X *( N−i )] W^ 1
(where W is the butterfly factor)
There are several variations on this technique including maintaining the original FFT size and then packing two real arrays into a single complex array; a simple post processing operation being used to separate the data. The technique is described in “Handbook of Real Time FFTs” by Winthrop Smith and Joanne Smith (IEEE press), the basic steps are:
Let:
a(n) and b(n) be real vectors of length N, let:
c ( n )= a ( n )+ jb ( n ) (where j is the square root of −1).
Let:
C ( k )= FFT[c ( n )]= R ( k )+ jI ( k ) where k= 0, 1, 2, . . . ( N− 1)
The complex transforms, A(k) and B(k), of the original vectors are now separated using, for example:
for (k = 1; k++,k <=(N−2)/2) {
RP(k) = RP(N−k) = (R(k) + R(N−k))/2
RM(k) = −RM(N−k) = (R(k) − R(N−k))/2
IP(k) = IP(N−k) = (I(k) + I(N−k)))/2
IM(k) = −IM(N−k) = (I(k) − I(N−k)))/2
}
RP(0) = R(0)
IP(0) = I(0)
RM(0) = IM(0) = RM(N/2) = IM(N/2) = 0
RP(N/2) = R(N/2)
IP(N/2) = I(N/2)
(where P and M are respectively..........please identify...)
Finally (and for example):
for (k = 0; k++, k <=(N−1)) {
A(k) = RP(k) + jIM(k)
B(k) = IP(k) − jRM(k)
}
Transforming two real arrays at the same time is potentially more efficient but overall the technique has the disadvantage that the overall latency for data is doubled. Some services, such as digitised voice, have strict latency requirements and this additional delay may be unacceptable.
SUMMARY OF THE INVENTION
The present invention seeks to avoid the latter disadvantage by exploiting a new technique which can be used to simplify the construction of a transceiver in an ADSL DMT system, but without compromising reliability.
Broadly speaking, the invention can be applied to a discrete multitone (DMT) and orthogonal frequency division multiplex (OFDM) transceiver wherein communication occurs between stations in the form of symbols. The symbols are distributed and transmitted in channels which are allocated when making a link between the stations, each channel supporting a number of bits depending on the spectral response of the link when it is established. Such a system has a transmit mode where, according to the channel allocations, variable length sequences of bits are encoded. With QAM, for example, these would be amplitude quadrature pairs. Inverse fast Fourier transforms (iFFT's) are normally performed (e.g. on the QAM pairs) before the symbols are transmitted. In a receive mode, the received symbols are sampled and fast Fourier transforms (FFT's) are normally performed on the samples to produce data sequences (e.g. QAM pairs) which are decoded into variable length sequences for each channel. However, instead of providing separate modules for performing iFFT's and FFT's, a transceiver incorporating the invention has only a single FFT, or iFFT which operates on real and imaginary parts of the data stream; the outputs of the FFT or iFFT being supplied to a post processing stage where simultaneous equations having real and imaginary terms for the transmit and receive data, are solved in order to separate the transmit and receive data.
For example, FFT's can be performed on the complex conjugate QAM pairs to produce the effect of iFFT's on the transmission data, whilst FFT's can also be performed on received QAM pairs, the real and imaginary parts being separated later by post processing. More particularly, where pairs of sample values output from a single FFT are of the form y[x]=P+jQ and y[N−x]=R+jS, a simple stage of post processing can be used to separate the transmit and receive data on the basis of solving:
A =( Q+S )/2
B =( Q−S )/2
Where,
rx data[ x]=A+jB
tx data [ x]=P−S and tx data [ N−x]=R−Q
An embodiment of the invention will now be described, by way of example, with reference to the accompanying schematic drawings, in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified diagram of a conventional xDSL modem;
FIG. 2 shows an embodiment of the invention; and
FIG. 3 shows a detail of part of the embodiment illustrated by FIG. 2 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , this illustrates, in a much simplified form, a conventional xDSL modem where separate iFFt's are performed on transmission data and FFT's are performed on reception data.
An input transmitted sample stream tx data is processed to produce symbols for transmission on the telephone line 7 . For example, variable-length sequences of bits (according to a table of channel bit allocations) are passed to QAM complex encoder 1 which then produces one amplitude pair per sequence of bits. The amplitude pairs are then processed by iFFT 2 , and parallel to serial converter 3 which creates a sample stream at some multiple of the symbol rate. This is then upsampled in filtering stage 4 and passed to DAC 5 to produce symbols for transmission. Hybrid circuit 8 allows either transmission, or reception of symbols on line 7 .
When symbols are received from the line 7 , these are processed in order to reproduce a received data stream rx, For example, a sequence of received symbols is sampled by the ADC 9 at a substantially fixed sampling rate to produce a stream of samples, which are then downsampled and passed through an equaliser (represented by filtering stage 10 ) and serial to parallel converter 11 before being processed by an FFT 12 (e.g. using n frequency bins, such that each carrier tone in the signal maps to a distinct frequency bin in the FFT). The output of the FFT 12 comprises a sequence of n pairs of amplitude in-phase and quadrature components (in each frequency bin), which are then processed (e.g. by a frequency domain equaliser, not shown) to correct for phase shifts before the amplitude pairs are fed into complex decoder 13 (which, using a table of carrier channel bit allocations, converts the amplitude pairs into variable-length sequences of bits using known QAM decoding techniques). Typically, the bits are then combined to produce an output stream of fixed-length data words.
The processing stages are usually implemented in hardware with a software controller overseeing the various stages. Hybrid stage 8 operates so as to transmit symbols or to receive symbols. All of the stages other than the ADC and DAC may alternatively be implemented solely or substantially in software, subject to the availability of sufficient processing power, or wholly or substantially in hardware.
In the system shown, 256 samples of data are processed by the iFFT, and 256 samples by FFT's. The number 256/512 indicates the number of values in use in a G.992.1 and G.992.2 system respectively. This can be the same in the preferred embodiment of the invention, or it can employ different sizes of FFT.
The diagram has been simplified to facilitate understanding, since the system would normally includes far more complex circuitry, for example, cyclic prefix and asymmetry between tx and rx data sizes are not discussed here, because they are well known and do not form part of the invention. Moreover, the operation of such an xDSL modem is well known in the art, ie. where separate FFT and iFFT is used respectively for steams of data to be transmitted and data which is received.
Referring now to FIG. 2 , where similar elements have been identified by similar reference numerals, an xDSL modem has only FFT 12 a , because this performs FFT's on complex tx data, and FFT's on rx data. In order to enable the use of one FFT, the tx data is supplied to the complex encoder 1, whereby complex conjugate tx[constx]* samples (256/512) are processed by the FFT 12 a and then separated from rx data in a post processing stage 14 , which solves simultaneous equations as explained below The output from stage 14 passes to a parallel to serial converter 3 and then through filters 4 and DAC 5 , before being supplied (as symbols) to the line 7 via hybrid circuitry 8 . The conjugate operation can be built into the transmit constellation generator before using the FFT, since it is not needed on the receive side, because FFT is correct for the received data.
Symbols received from the line 7 likewise pass through the hybrid circuitry 8 to ADC 9 whereby the data stream is filtered 10 and then supplied to serial to parallel converter 11 . Output values are multiplied by (1+j) in multiplier 15 and then supplied by adder 16 to FFT 11 a . This enables rx samples to be separated later from the tx samples in the post processing stage 15 , where simultaneous equations are solved to derive parameters for separating rx data samples (128/256) that are then decoded in the complex decoder 13 . The separation of the data from the single FFT produces N/2 complex values for the receive constellation and N real values as the transmit data. Moreover, in a real application, there is freedom over scheduling of the FFT operations by inserting queues of samples in series with the transmit and receive filters. These queues keep the flow of samples at the DAC and ADC steady, but relax FFT timing.
The operation of this post processing stage will be more apparent from the following analysis:
Assuming that txconst[x] is the complex transmit data from the QAM or similar modulator and RX[x] is the real received data, we can form:
tx data[ x]=tx const*[ x]
where * is the complex conjugate. This operation is required because we actually need the transmit data to be operated on by an iFFT and this is done by operating an FFT on the complex conjugate of the original data.
We also form:
p[x]=tx data[ x]+RX[x]+jRX[x]
and by taking the FFT:
y[x]=FFT ( p[x ])= FFT ( tx data[ x]+RX[x]+jRX[x ])= FFT ( tx data[ x ])+ FFT ( RX[x ])+ jFFT[x]
If:
tx[x]=FFT ( tx data[ x ])
rx const[ x]=FFT ( RX[x ])= A+jB
therefore:
y[x]=tx[x]+rx const[ x]+jrx const[x]
Considering the values of y[x] at the locations (x) and (N−x) where N is the size of the Fourier transform, then:
y[x]=P+jQ=tx[x]+A+jB+jA−B
y[N−x]=R+jS=tx[N−x]+A−jB+jA+B
because the receive data was real valued only.
So,
P=tx[x]+A−B
Q=A+B
R=tx[N−x]+A+B
S=A−B
Solving for the variables on the right hand side we have:
tx[x]=P−S
tx[N−x]=R−Q
Also,
A =( Q+S )/2
B =( Q−S )/2
Whereby,
rx const[ x]=A+jB
Thus a single post processing stage can be constructed as shown in FIG. 3 to separate the transmit and receive data. In this processing stage, the output from the FFT is shown as y[x]=P+jQ and y[N−x]=R+jS. Imaginary parts jQ and jS are added in adder 17 and the result is divided by 2 in divider 18 to yield (Q+S)/2=A. Similarly, the imaginary parts jQ and jS are subtracted (by adding jQ to −jS in adder 19) and the result is divided by 2 in divider 20 to yield (Q−S)/2=B. The complex receive data rxconst(x) can then be derived from A+jB. By analogy, it can be seen that adders 21 and 22 are used to provide txdata[x]=P−S and txdata[N−x]=R−Q, from which transmission data can be derived. The set of operations is clearly symmetric and we could, to minimise the post processing, choose to use an iFFT instead of an FFT.
In many ADSL implementations the transmit iFFT and receive FFT are of different lengths and further post processing is required to perform the sample rate conversion so that the ADC and DAC have the same sample rate. A further advantage of this technique is that it eliminates this sample rate conversion step. Where the inverse process is used, i.e. where the circuitry shown in FIG. 2 includes an iFFT stage (not shown) rather than the FFT stage, the construction and operation will be clear to those skilled in the art.
Overall, the technique eliminates either the FFT or iFFT, substitutes a simple single pass post processing operation, and eliminates the sample rate conversion process. All of which result in a considerable reduction in computational complexity. | A DMT/OFDM transceiver wherein communication occurs between stations in the form of symbols distributed and transmitted in channels which are allocated when making a link between the stations, each channel supporting a number of bits depending on the spectral response of the link when established. Instead of providing separate modules for performing iFFT's and FFT's, the transceiver has only a single FFT, or iFFT which operates on real and imaginary parts of the data stream; the outputs of the FFT or iFFT being supplied to a post processing stage where simultaneous equations having real and imaginary terms for the transmit and receive data, are solved in order to separate the transmit and receive data. | 7 |
BACKGROUND OF THE APPLICATION
This invention relates to lighter-than-air aircraft, and in particular to such an aircraft which is stable and highly maneuverable.
Lighter-than-air or buoyant aircraft typically include a balloon section, a means of propulsion, and a body section or fuselage carried beneath the balloon. Lighter-than-air aircraft have the advantage that they take little energy to ascend, and little energy to propel. Thus, in comparison to airplanes or helicopters, for example, lighter-than-air aircraft require less fuel to operate.
In lighter-than-air aircraft which do include propulsion means (hot air balloons are generally void of any propulsion means) the propulsion means is typically fixed to the balloon portion of the aircraft. This prevents the aircraft from being able to turn without moving in a horizontal plane, that is, the aircraft cannot turn in place. Further, the aircraft may not be as stable is it could be.
SUMMARY OF THE INVENTION
One object of the present invention is to provide an improved lighter-than-air aircraft.
Another object is to provide such an aircraft which is highly maneuverable.
Another object is to provide such an aircraft which is stable.
Another object is to provide such an aircraft in which the propulsion section is separate from and depends from the balloon section of the aircraft.
These and other objects will become apparent to those skilled in the art in light of the following disclosure and accompanying drawings.
In accordance with the invention, generally stated, a stable and highly maneuverable lighter-than-air aircraft is provided. The aircraft includes a body portion which is supported beneath a balloon portion by a stem or axle. The balloon is fillable with a lighter-than-air gas and is sized to accept sufficient amounts of gas to make the aircraft buoyant. The balloon portion is rotationally fixed to the axle and the axle is rotationally journaled in the body. Thus, the balloon portion can rotate relative to the body portion. A motor is housed in the body portion and is operable to propel the aircraft in a desired direction. The aircraft is operated such that the balloon portion rotates above the body portion without rotating the body portion. The rotation of the balloon portion provides stability to the aircraft and the ability for the body portion to rotate about the axle enables the aircraft to be highly maneuverable.
The body portion includes an air inlet, a rear thruster, and two side thrusters. The motor, which is preferably an impeller or jet motor, is operable to draw air in through the air inlet and to expel the air out the thrusters to propel the aircraft along a desired vector. The side thrusters each include an outlet and are operable to alter an angle of the outlet relative to the horizontal to alter the altitude of the aircraft. A rudder is pivotally mounted in the rear thruster to alter the direction of travel of the aircraft. Servomechanisms are provided to pivot the rudder and change the angle of the side thruster outlets. Preferably, the side thruster outlets are pivoted in unison so that they will always direct air along substantially the same vector.
As noted, the motor drives an impeller. The motor is rotationally fixed to the axle and the axle and impeller are on opposite sides of the motor. Thus, as the impeller rotates, it creates a counter-rotation in the motor which is passed to the balloon portion through the axle. Because the axle is rotatably journaled in the body portion, no counter rotation is induced in the body portion, and the body portion remains substantially positionally fixed. That is, the body portion only rotates when the rudder is operated to rotate the body to alter the direction of travel of the aircraft.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a lighter-than-air aircraft of the present invention;
FIG. 2 is a perspective view of a body portion of the aircraft;
FIG. 3 is a top plan view of the aircraft, less the balloon;
FIG. 4 is a bottom plan view of the aircraft;
FIG. 5 is a cross-sectional view taken along line 5--5 of FIG. 4;
FIG. 6 is a cross-sectional view of the housing showing the manner of mounting of the housing on the motor;
FIG. 7 is a perspective view of a side thruster of the aircraft; and
FIG. 8 is a perspective view of a rear thruster of the aircraft.
DESCRIPTION OF THE PREFERRED EMBODIMENT
A lighter than air aircraft 1 of the present invention is shown generally in FIG. 1. The aircraft 1 includes a body portion 3 suspended from a balloon 5 by a stem or axle 7. The balloon 5 includes a skin or membrane 9 having an opening 11 (FIG. 4) at a bottom of the balloon. The balloon is filled with a gas which is lighter than air, for example helium, and is sized so that there is sufficient helium to off-set the weight of the body portion 3 and balloon 5 so that the aircraft 1 will be buoyant. Other gases, for example, hot air, could also be used.
The stem or axle 7 is secured to the top of a motor 13 (FIG. 6) which is contained within the body 3. The motor 13 shown is a gas powered motor, but may be any type of motor. For example, the motor may an electric or jet motor. The motor 13 includes an impeller 15 which is rotated by the motor to propel the aircraft 1, as will be described below. The axle 7 is fixed to the top of the motor. The motor 13 preferably includes a post 17 which extends upwardly from a mounting plate 16. The axle 7 is preferably hollow (at least at the bottom thereof) and is slid over the post 17. The post 17 and axle 7 include aligned pin holes 18 and 20, respectively, which accept a pin 19, such as a cotter pin, to secure the axle 7 to the post 17. The axle 7 thus cannot rotate with respect to the motor 13. Preferably, a ring 21 is mounted around the axle 7 at the level of the pin holes. The pin 19 thus passes through the ring 21 to hold the ring in place relative to the axle.
A hub 25 is formed or mounted at the top of the axle 7. A plurality of evenly spaced apart spokes 27 (FIG. 3) (three spokes are shown) extend outwardly from the hub. Preferably, the hub 25 includes bosses 29 (FIG. 6) which telescopically receive the spokes 27. The balloon 5 has sleeves 31 (FIGS. 4 and 5) which receive the spokes 27 to connect the balloon 5 to the axle 7. The sleeves 31 are formed of strips of elongate material which are connected to the outer skin 9 of the balloon 5 along their elongate sides. The sleeves 31 are preferably open at their ends. To mount the balloon 5 to the axle 7, the spokes 27 are passed through the balloon sleeves 31 and into the hub bosses 29. The hub 25 is fixed to the axle 7 so that the hub cannot rotate relative to the axle.
The body 3 includes a housing or manifold 35 (FIGS. 2 and 6) having a top surface 37, sides 39, and a generally opened bottom 41. The top surface 37 has an opening 43 through which the axle 7 extends. The manifold is not secured to the axle, but rather, rests on the ring 21. The axle 7 and the manifold 35 can thus pivot or rotate with respect to each other. If desired, a bearing 45 can be positioned between the edge of the opening 43 and the axle 7 to facilitate the pivotability of the manifold with respect to the axle 7. To center the axle 7 within manifold 35 so that it extends through the center of opening 43, a spider 44 having a central opening and a plurality of legs is secured to the top surface 37 of the manifold 35. The axle then extends through the opening in the spider 44, and the spider sits on the bearing 45.
The bottom 41 has an opening 47 which defines an air inlet to the manifold, and the sides 39 have three outlets: one back outlet 49 and two side outlets 51. As can be appreciated, the impeller 15 is spun by the motor in a direction that will bring air into the housing or manifold 35 and then will force the air out the outlets 49 and 51.
The rear outlet 49 has a tube 53 rotatably mounted thereto to define a rear thruster. The air expelled out the rear thruster will give the aircraft 1 forward momentum. A rudder 55 is pivotally mounted at the back of the tube 53 and is operable to be selectively pivoted. Thus, the direction of forward travel of the aircraft 1 can be controlled.
Second and third tubes 57 and 59 extend from the side outlets 51 and are rotatably connected to the manifold 35 at the outlets to define side thrusters. The tubes 57 and 59 are identical. Each tube includes a bend or elbow 60 so that the outlet 61 of the tube will face generally rearwardly. Because the tubes are rotatably mounted to the body, the tubes can be rotated such that the outlet 61 will face generally above or below a horizontal plane. The thrust provided by the air passing out of the tubes 57 and 59 can be used to change the elevation of the aircraft 1. A axial plate or flange 63 extends around the tube and passes in front of the outlet 61. The flange 63 is formed or mounted on the tube to extend along the center of the tube. That is, it lies on a diameter of the tube. As noted, the flange 63 extends across the opening 61 of the tubes 57 and 59. The portion 65 of the flange 63 which passes across the opening 61 is enlarged, as can be seen in FIGS. 3 and 4. The flange portion 65 forms, in a sense, an immobile rudder which will help direct the flow of air out of the side thrusters 57 and 59.
Servomechanisms are provided to pivot the rudder 55 and rotate the side thrusters 57 and 59. A rear servomechanism 71 (FIG. 8) is mounted to the outside of the housing 35 above the rear outlet 49. A pivot plate 73 is connected to, and extends from, the servomechanism 71, such that when the servomechanism is activated, the plate will pivot in a selected direction (either clockwise or counter-clockwise) about an axis a desired amount. A tiller 75 is mounted to, and extends from the rudder 55 at a right angle thereto. A rod 77 is pivotally connected at one end to the pivot plate 73 and at another end to the tiller 75. The servomechanism is operated, as noted, to selectively pivot the pivot plate 73. As the pivot plate is turned or pivoted, the rod 77 will be pulled or pushed, resulting in pivoting of the rudder. The direction of movement of the aircraft can thus be selectively controlled.
Second and third servomechanisms 81 (FIG. 7) are mounted to the housing 35 above the side outlets 51. Pivot plates 83 are connected to the servomechanisms 81 to be pivoted thereby in the same manner as pivot plate 73. The plates 83 extend beyond either side of the servomechanisms 81 so that have two free ends. Rods 85 extend between and are pivotally connected to the ends of pivot plates 83 and the flange 63 of the thrusters 57 and 59. Preferably, there are two rods 85 for each thruster to facilitate rotation of the thruster. One rod is connected to either side of the thruster, as can be seen in FIG. 7. As with the rudder, when the servomechanisms 81 are operated to pivot the plates 83, each plate pulls one rod 85 and pushes the other. Thus, a plate pulls one side of the thruster upwardly and pushes the other side of the thruster downwardly to pivot the thruster. Preferably, the side thrusters are controlled in unison so that the outlets 61 will always face substantially the same direction (i.e., are at the same angle to the horizontal). Thus, one of the thrusters will not, for example, be generating a downward thrust while the other is generating an upward thrust, or for that matter, the two side thrusters will not be generating thrusts along two different vectors.
As noted above, the manifold 35 is not fixed to the axle 7. Rather, it can rotate about the axle 7. As the impeller 15 is rotated, it will generate a counter-rotation in the motor 13 in much the same way a helicopter rotor causes the fuselage of the helicopter to rotate when the tail rotor of the helicopter is not operating. The counter-rotation induced in the motor is passed on to the balloon 5 through the axle 7 and spokes 27. Thus, as the aircraft 1 is operated, the balloon spins or rotates on its axis in a rotational direction opposite that of the impeller. The spinning of the balloon will give the aircraft more stability, in the same way a spinning top is stabilized by rotation of the top. Because the housing 35 is not fixed to the axle 7, rotation that is passed to the balloon will not cause the housing to rotate.
Further, because the manifold or housing 35 rotates about the axle, the aircraft can be rotated in place. That is, it can turn a complete circle without requiring any forward momentum. Thus, by selective operation of the rudder, the manifold 35 can be rotated 180° to stop the forward motion of the aircraft. The ability for the housing to rotate about the axle similarly allows the aircraft to turn with substantially no forward motion. The aircraft 1 is thus highly maneuverable.
As variations within the scope of the appended claims may be apparent to those skilled in the art, the foregoing description is set forth only for illustrative purposes and is not meant to be limiting. For example, mechanisms other than servomechanisms can be provided to pivot the rudder and rotate the side thrusters. Pulley systems or pneumatic systems could be used in place of the servomechanism. More than three spokes can be used to connect the balloon to the hub. The spokes can be fixed directly to the hub, or can be telescopically received in bores in the hub. Other mechanisms, other than impeller induced counter-rotation can be used to rotate the balloon. For example, a gearing or pulley system can be used to rotate the balloon. This gearing or pulley system could be driven by the same motor which propels the aircraft, or a second motor could be provided to drive the gearing or pulley system. Other means could be used to mount the axle to the motor. For example, the axle could be welded to the motor mount. Because the side thruster create a generally forward thrust in their own right, the rear thruster could be removed and the rear outlet closed. The rudder could simply be mounted to the rear of the body portion, or rudders could be mounted in the outlets of the side thrusters. These examples are merely illustrative. | A stable and highly maneuverable lighter-than-air aircraft is provided. The aircraft includes a body portion which is supported beneath a balloon portion by a stem or axle. The balloon is fillable with a lighter-than-air gas and is sized to accept sufficient amounts of gas to make the aircraft buoyant. The balloon portion is rotationally fixed to the axle and the axle is rotationally journaled in the body. Thus, the balloon portion can rotate relative to the body portion and the body can selectively be rotated relative to the axle. A motor is housed in the body portion and is operable to propel the aircraft in a desired direction. The aircraft is operated such that the balloon portion rotates above the body portion without rotating the body portion. The rotation of the balloon portion provides stability to the aircraft and the ability for the body portion to rotate about the axle enables the aircraft to be highly maneuverable. | 1 |
CROSS REFERENCE TO RELATED APPLICATION
[0001] This application claims priority under 35 U.S.C. §119(e) to Chinese Patent Application Nos. CN201210055616.X, filed Mar. 5, 2012, and CN201210055620.6, filed Mar. 5, 2012.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a resin article, particularly to a composite formulation for a recycled EVA (ethylene-vinyl acetate copolymer), a recycled PP (chlorinated polypropylene), a recycled PVC (polyvinyl chloride), and a recycled PE (polyethylene), as well as to a process for the heat-pressing of a recycled plastic composite.
[0004] 2. Background Information
[0005] Currently the problem in the resin article and the related art is the high cost of the raw material, the blank will be modified by the repairing, low production efficiency, the repeated usage of the corresponding mold being limited (about 300 times), and the lower surface smoothness, heat resistance, and toughness of the resin article.
SUMMARY OF THE INVENTION
[0006] The present invention provides a formulation for a recycled plastic composite comprising in the terms of weight percent: recycled EVA plastic from 30% to 80%, a stone powder from 20% to 70%. Preferably, said formulation comprises in the terms of weight percent: the recycled EVA plastic greater than 70% and less than or equal to 80%, the stone powder greater than or equal to 20% and less than 30%. The recycled plastic comprises a recycled EVA (ethylene-vinyl acetate copolymer), a recycled PP (chlorinated polypropylene), a recycled PVC (polyvinyl chloride), and a recycled PE (polyethylene). The formulation for the recycled plastic composite of the present invention can improve the toughness, strength, surface smoothness, heat resistance, and electroplating performance of various products obtained, can be pressed through hydraulic press, results in the increased production, lowered labor, cost for producing various products and decreased pollution.
[0007] The present invention further provides a process for the heat-pressing of a recycled plastic composite comprising sufficiently mixing the pellet of the recycled plastic and the heavy calcium carbonate according to the formulations to get the composite, the composite is fed to a screw melting machine with electric heating, heated and further mixed, the thick composite after being heated is conveyed to the outlet by the screw; the thick composite is obtained at the outlet, conveyed to the steel mold of the hydraulic press according to the volume of the mold to be molded and pressed strongly; said thick composite is cooled in the steel mold for 5 minute to 15 minute with the recirculation of the cooling water to de-mold the thick composite, and the thick composite is completely immersed in the water to be cooled completely to finish the heat-pressing of the composite. The process of heat-pressing the composite of the present invention can improve production efficiency, the surface smoothness, the toughness of the product, the saving of the raw material, improving the heat resistance from −40° C. to −80° C., improve the electroplating performance of various products obtained, results in the decreased pollution.
[0008] More specifically, the present invention provides a formulation for the recycled plastic composite which can improve the toughness, strength, surface smoothness, heat resistance, and electroplating performance of various products obtained, results in the increased production, lowered labor, cost for producing various products and decreased pollution. In order to achieve the subject of the present invention, there is provided the following embodiments: a formulation for a recycled plastic composite comprising in the terms of weight percent: a recycled plastic from 30% to 80%, a heavy calcium carbonate from 20% to 70%.
[0009] Preferably, the recycled plastic is one or mixture of more in any ratio of a recycled EVA (ethylene-vinyl acetate copolymer), a recycled PP (chlorinated polypropylene), a recycled PVC (polyvinyl chloride), and a recycled PE (polyethylene). In one embodiment, said formulation comprises in the terms of weight percent: the recycled plastic greater than 70% and less than or equal to 80%, the heavy calcium carbonate greater than or equal to 20% and less than 30%. In one embodiment, said formulation comprises in the terms of weight percent: the recycled plastic greater than 60% and less than or equal to 70%, the heavy calcium carbonate greater than or equal to 30% and less than 40%. In one embodiment, said formulation comprises in the terms of weight percent: the recycled plastic greater than 50% and less than or equal to 60%, the heavy calcium carbonate greater than or equal to 40% and less than 50%. In one embodiment, said formulation comprises in the terms of weight percent: the recycled plastic greater than 40% and less than or equal to 50%, the heavy calcium carbonate greater than or equal to 50% and less than 60%. In one embodiment, said formulation comprises in the terms of weight percent: the recycled plastic greater than 30% and less than or equal to 40%, the heavy calcium carbonate greater than or equal to 60% and less than 70%. In one embodiment, the talc can be added to any of the formulation in an amount from 1% to 15%.
[0010] The technical effects achieved in the present invention through the above mentioned embodiments include improving the toughness, strength, surface smoothness, heat resistance, and electroplating performance of various products obtained, can be pressed through hydraulic press, results in the increased production, lowered labor, cost for producing various products and decreased pollution.
[0011] Further, the present invention provides a process of heat-pressing the composite which can improve production efficiency, the surface smoothness, the toughness of the product, the saving of the raw material, improving the heat resistance from −40° C. to −80° C., improve the electroplating performance of various products obtained, results in the decreased pollution. In order to achieve the subject of the present invention, there is provided a process for the heat-pressing of a recycled plastic composite comprising the steps of:
[0012] A. sufficiently mixing the pellet of the recycled plastic and the heavy calcium carbonate according to the formulations to get the composite;
[0013] B. the composite is fed to a screw melting machine with electric heating, heated and further mixed, the thick composite after being heated is conveyed to the outlet by the screw;
[0014] C. the thick composite is obtained at the outlet, conveyed to the steel mold of the hydraulic press according to the volume of the mold to be molded and pressed strongly;
[0015] D. said thick composite is cooled in the steel mold for 5 minute to 15 minute with the recirculation of the cooling water to de-mold the thick composite, and the thick composite is completely immersed in the water to be cooled completely to finish the heat-pressing of the composite.
[0000] Preferably, the size of the heavy calcium carbonate is from 600 mesh to 1200 mesh. Preferably, the temperature in the screw melting machine with electric heating is controlled to be from 160° C. to 240° C.
[0016] The technical effects achieved in the present invention through the above mentioned embodiments include improving production efficiency, the surface smoothness, the toughness of the product, the saving of the raw material, improving the heat resistance from −40° C. to −80° C., improving the electroplating performance of various products obtained, resulting in the decreased pollution. The product of the process of the present invention is the resin article such as flowerpot, frame for the image, lamp bracket and lamp socket, fence of the garden, guard of the garden, gift, furniture decoration, construction decoration, graving article, graving of emulation, and the raw materials for emulation animal and plant graving.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] The present invention provides a formulation for a recycled plastic composite comprising in the terms of weight percent: a recycled EVA plastic from 30% to 80%, a heavy calcium carbonate from 20% to 70%.
[0018] Preferably, the recycled plastic is one or mixture of more in any ratio of a recycled EVA (ethylene-vinyl acetate copolymer), a recycled PP (chlorinated polypropylene), a recycled PVC (polyvinyl chloride), and a recycled PE (polyethylene). Specifically the formulation for the high toughness recycled plastic composite comprises in the terms of weight percent: the recycled plastic greater than 70% and less than or equal to 80%, the heavy calcium carbonate greater than or equal to 20% and less than 30%.
[0019] Formulation 1: the recycled plastic 80%, the heavy calcium carbonate 20%.
[0020] Formulation 2: the recycled plastic 71%, the heavy calcium carbonate 29%.
[0021] Formulation 3: the recycled plastic 75%, the heavy calcium carbonate 25%.
[0022] More specifically the formulation for the less high toughness recycled plastic composite comprises in the terms of weight percent: the recycled plastic greater than 60% and less than or equal to 70%, the heavy calcium carbonate greater than or equal to 30% and less than 40%.
[0023] Formulation 4: the recycled EVA plastic 70%, the heavy calcium carbonate 30%.
[0024] Formulation 5: the recycled EVA plastic 65%, the heavy calcium carbonate 35%.
[0025] Formulation 6: the recycled EVA plastic 61%, the heavy calcium carbonate 39%.
[0026] Still more specifically the formulation for the medium toughness recycled plastic composite comprises in the terms of weight percent: the recycled plastic greater than 50% and less than or equal to 60%, the heavy calcium carbonate greater than or equal to 40% and less than 50%.
[0027] Formulation 7: the recycled EVA plastic 60%, the heavy calcium carbonate 40%.
[0028] Formulation 8: the recycled EVA plastic 55%, the heavy calcium carbonate 45%.
[0029] Formulation 9: the recycled EVA plastic 51% the heavy calcium carbonate 49%.
[0030] Still more specifically the formulation for the less medium toughness recycled plastic composite comprises in the terms of weight percent: the recycled plastic greater than 40% and less than or equal to 50%, the heavy calcium carbonate greater than or equal to 50% and less than 60%.
[0031] Formulation 10: the recycled EVA plastic 50%, the heavy calcium carbonate 50%.
[0032] Formulation 11: the recycled EVA plastic 45%, the heavy calcium carbonate 55%.
[0033] Formulation 12: the recycled EVA plastic 39%, the heavy calcium carbonate 61%.
[0034] Still more specifically the formulation for the low toughness recycled plastic composite comprises in the terms of weight percent: the recycled plastic greater than 30% and less than or equal to 40%, the heavy calcium carbonate greater than or equal to 60% and less than 70%.
[0035] Formulation 13: the recycled EVA plastic 40%, the heavy calcium carbonate 60%.
[0036] Formulation 14: the recycled EVA plastic 35%, the heavy calcium carbonate 65%.
[0037] Formulation 15: the recycled EVA plastic 31%, the heavy calcium carbonate 69%.
[0038] Preferably, the talc can be added to any of the formulation in an amount from 1% to 15% in order to improve the surface smoothness of the article.
[0039] The method for producing the composite comprises sufficiently mixing the pellet of the recycled plastic and the heavy calcium carbonate according to any abovementioned formulations to get the composite, the composite is fed to a screw melting machine with electric heating, heated and further mixed, the thick composite after being heated is conveyed to the outlet by the screw; the thick composite is obtained at the outlet, conveyed to the steel mold of the hydraulic press according to the volume of the mold to be molded, the thick composite is completely immersed in the water after cooling the temperature thereof to complete the heat-pressing of the composite. The formulation of the present invention is useful in the resin article such as for the manufacturing of flowerpot, frame for the image, lamp bracket and lamp socket, fence of the garden, guard of the garden, unsaturated resin article, gift, furniture decoration, construction decoration, graving article, graving of emulation, and the raw materials for various products.
[0040] The present invention provides a process for the heat-pressing of a recycled plastic composite comprising the steps of:
[0041] A. sufficiently mixing the pellet of the recycled plastic and the heavy calcium carbonate according to the formulations to get the composite wherein the mixing can be carried out through a manual or mechanical means. The recycled plastic is one or mixture of more in any ratio of a recycled EVA (ethylene-vinyl acetate copolymer), a recycled PP (chlorinated polypropylene), a recycled PVC (polyvinyl chloride), and a recycled PE (polyethylene). The formulation is as follows:
[0042] The formulation for the high toughness recycled plastic composite: the recycled plastic from 70% to 80%, the heavy calcium carbonate from 20% to 30%; the formulation for the less high toughness recycled plastic: the recycled plastic from 60% to 70%, the heavy calcium carbonate from 30% to 40%; the formulation for the medium toughness recycled plastic: the recycled plastic from 50% to 60%, the heavy calcium carbonate from 40% to 50%; the formulation for the less medium toughness recycled plastic: the recycled plastic from 40% to 50%, the heavy calcium carbonate from 50% to 60%; the formulation for the low toughness recycled plastic: the recycled plastic from 30% to 40%, the heavy calcium carbonate from 60% to 70%.
[0043] B. the composite is fed to a screw melting machine with electric, heating, heated and further mixed, the thick composite after being, heated is conveyed to the outlet by the screw; in the step B, the feeding of the composite to the screw melting machine with electric heating can be carried out through a manual or mechanical means;
[0044] C. the thick composite is obtained at the outlet, conveyed to the steel mold of the hydraulic press according, to the volume of the mold to be molded and pressed strongly; in the step C, the obtaining of the thick composite can be carried out through a manual or mechanical means; or the conveying of the thick composite to the steel mold of the hydraulic press can be carried out through a manual or mechanical means;
[0045] D. said thick composite is cooled in the steel mold for 5 minute to 15 minute with the recirculation of the cooling water to de-mold the thick composite, and the thick composite is completely immersed in the water to be cooled completely to finish the heat-pressing of the composite.
[0046] Preferably in the example described above, the size of the heavy calcium carbonate is from 600 mesh to 1200 mesh. Preferably in the example described above, the temperature in the screw melting, machine with electric heating is controlled to be from 160° C. to 240° C.
[0047] While specific embodiments of the invention have been described in detail, it will be appreciated by those skilled in the art that various modifications and alternatives to those details could be developed in light of the overall teachings of the disclosure. Accordingly, the particular arrangements disclosed are meant to be illustrative only and not limiting as to the scope of invention which is to be given the full breadth of the claims appended and any and all equivalents thereof. | A formulation for a recycled plastic, composite composition, and a method of making the composite composition, is provided. The composite composition includes recycled EVA plastic from 30% to 80%, a stone powder from 20% to 70%; percentages by weight. | 2 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a vehicle speed control system for controlling vehicle speeds by controlling either or both of the displacement of the hydraulic pump and hydraulic motor in the hydraulic transmission.
2. Description of the Prior Art
A conventional hydraulic transmission typically has a variable capacity hydraulic pump (e.g. swash plate type pump) to be driven by an engine on the engine side and a variable capacity hydraulic motor (swash plate type motor) on the driving shaft side for driving vehicle wheels or a crawler belt, and transmits the driving force of the engine to the wheels or the crawler belt by directing the operating fluid discharged from the pump through the hydraulic piping. Speed control of the vehicle is performed by adjusting the discharge amount of the hydraulic pump and the suction amount of the hydraulic motor per rotation of the engine by means of controlling the slope angle of both the swash plates of the hydraulic pump and the hydraulic motor, thereby changing the speed of the driving shaft for each rotation of the engine.
Since the conventional vehicle speed control system is designed to perform vehicle speed control by mechanically controlling the slope angle of the swash plate by the movement caused by the operation of a vehicle speed setting lever, a brake lever and a throttle lever by the vehicle operator, the structure of the control system becomes unavoidably complex. Accordingly, in the conventional system performing vehicle speed control is difficult and therefore driving comfort, safety and other factors are likely to be neglected.
SUMMARY OF THE INVENTION
Accordingly, the present invention has been made to solve the problems involved in the prior art, and an object of the present invention is to provide a vehicle speed control system which assures comfortable driving, smooth vehicle speed control, and outstandingly safe vehicle speed control.
Another object of the present invention is to provide a vehicle speed control system wherein optimum delay characteristic is imparted to a vehicle speed command in accordance with whether the vehicle speed command is an acceleration command or a deceleration command, whereby a proper acceleration feeling can be felt during an acceleration period, while a shock caused by deceleration can be avoided during a deceleration period.
A further object of the present invention is to provide a vehicle speed control system wherein the speed control at the time from forward to backward travel or vice versa is performed smoothly as a result of provision of a switch before the feedback system which is transferred according to whether or not the vehicle speed command is in a dead area.
A still further object of the present invention is to provide a vehicle speed control system wherein whether the vehicle is running or in the stop state can be easily judged, hence promoting the travel safety, since the step-up quantity can be suitably adjusted when the vehicle speed command is out of the dead area.
A still further object of the present invention is to provide a vehicle speed control system wherein a desired braking is effected by suitably using the engine brake and mechanical brake according to the reduction of the vehicle speed command, or using both.
According to the present invention, a vehicle speed command set corresponding to the position of a vehicle speed setting lever is fed into a dead area setting circuit in which the value of the vehicle speed command is changed to be not smaller than a preset minimum speed of the vehicle when it falls out of the dead area. Then the command is supplied into different delay compensating circuits depending on whether it is an acceleration command or a deceleration command. Further, the command outputted from the delay compensating circuit is subtracted by a brake signal generated by the operation of a brake pedal. The command thus subtracted causes a mechanical brake signal to generate when the speed of the vehicle is zero or minus.
The present invention will be described in detail with reference to the attached drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic drawing showing an embodiment of the drive system to which the vehicle speed control system of the present invention applies;
FIG. 2 is a block diagram showing an embodiment of the control circuit of the present invention; and
FIG. 3 is a circuit diagram of an embodiment of the vehicle speed control arithmetic circuit of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, a hydraulic transmission 10 comprises a variable capacity hydraulic pump (hereinafter referred to simply as a hydraulic pump 11 and a variable capacity hydraulic motor (hereinafter referred to simply as a hydraulic motor) 12. The hydraulic pump 11 and the hydraulic motor 12 are connected to each other through hydraulic pipes 13a and 13b. A shaft 11a of the hydraulic pump 11 is coupled with the output shaft 1a of an engine 1, and is driven by the engine 1. A shaft 12a of the hydraulic motor 12 is coupled with driving wheels of a vehicle not shown to drive the wheels.
The variable capacity hydraulic pump is suitable for the use in the fixed output shaft torque, while the variable capacity hydraulic motor is suitable for the use in the fixed output. In this embodiment, both the hydraulic pump 11 and the hydraulic motor 12 are of the variable capacity type to exploit features of the both. In addition, the hydraulic pump 11 and the hydraulic motor 12 are a variable capacity type pump and variable capacity type motor that can change the displacement by changing the slope angles of swash plates 11b and 12b.
A pump swash plate servo unit 14 is for controlling the direction and amount of the discharge of hydraulic fluid of the hydraulic pump 11, and controls the direction and angle of the slope of the swash plate 11b according to the polarity and magnitude of a pump capacity change signal Sp from a control unit 20. The hydraulic pump 11 discharges the hydraulic fluid in the direction and at a flowrate corresponding to the slope direction and slope angle of the swash plate 11b. A motor swash plate servo unit 15 is for controlling the suction amount of hydraulic fluid of the hydraulic motor 12, and is designed to control the slope angle of the swash plate 12b of the hydraulic motor 12 based on a motor capacity change signal Sm from the control unit 20. The rotational direction and the torque of the hydraulic motor 12 change according to the direction and amount (suction amount) of entering hydraulic fluid. Accordingly, by controlling the discharge amount from the hydraulic pump 11 and the suction amount into the hydraulic motor 12, speed change control by the transmission 10 can be accomplished.
The control circuit 20 generates a pump capacity change signal Sp and a motor capacity change signal Sm for controlling the capacities of hydraulic pump 11 and hydraulic motor 12 as well as a mechanical brake signal Sb for controlling a mechanical brake 6 based on a signal corresponding to the position of a vehicle speed setting lever 2 for setting the vehicle speed which is generated by a potentiometer 21, a signal corresponding to the position of a brake pedal 3 which is generated by a potentiometer 22, a signal corresponding to the position of a throttle lever 4, and a pulse signal corresponding to the speed (rpm) of the engine 1 which is generated by an engine speed sensor 5.
The control circuit 20 will now be described with reference to the block diagram of FIG. 2. The control circuit 20 includes a vehicle speed control arithmetic circuit 30 to which signals from the potentiometers 21 and 22 are fed, an automatic speed change arithmetic circuit 40 to which signals are fed from the potentiometer 23 and the engine speed sensor 5, a servo drive circuit 50, and other elements.
The vehicle speed control arithmetic circuit 30 (the detail will be given later) comprises a dead area setting circuit 31, a compensating circuit 32, an absolute value circuit 33, a comparator 34, a discriminating circuit 35, a brake signal compensating circuit 36, and other elements. The dead area setting circuit 31 sets the dead area of a signal to be fed from the potentiometer 21, and also sets a step-up value so as to rise or fall by a specified value when the input signal falls out of the set dead area. The compensating circuit 32 outputs a signal in response to a signal supplied from the dead area setting circuit 31 with a suitable time delay, applying it to the absolute value circuit 33 and the discriminating circuit 35. The discriminating circuit 35 detects the polarity (positive or negative) of the input signal, and outputs a direction signal KFR which becomes "1" when the signal is positive, and "-1" when the signal is negative. The absolute value circuit 33 takes the absolute value of the input signal, and applies it to a subtracting point 37.
On the other hand, the brake signal compensating circuit 36 outputs a suitable brake signal according to the signal fed from the potentiometer 22, outputs the signal fed from the potentiometer 22 with a time delay, and outputs the signal as a brake signal Sb instantly when the input signal has exceeded a preset level. The brake signal Sb is applied to the subtracting point 37. At the subtracting point 37, the brake signal is subtracted from the signal fed from the absolute value circuit 33, and outputs the resultant signal to the comparator 34 and a subtracting point 51 as a vehicle speed command signal Vs.
When the vehicle speed command signal Vs becomes a value lower than vehicle speed "0", the comparator 34 outputs a signal "1" to the reset terminal R of a flip-flop 52 and to a coil 54a of a brake solenoid valve 54, thereby resetting the flip-flop 52, and actuating the mechanical brake 6 (see FIG. 1). A charge pressure switch 55 is for detecting that the charge pressure of the hydraulic transmission dropped below a specified pressure, and outputs a signal "1" to the set terminal S of the flip-flop upon the detection thereof. When set by the output of the switch 55, the flip-flop 52 outputs a signal "1" to the coil 54a of the brake solenoid valve 54 via an OR circuit 53 and also to a switch 56. As the signal "1" is fed, the switch 56 opens its contact so as to keep a vehicle speed command from being output to the servo drive circuit 50.
To the other input of the subtracting point 51, a speed change signal Sf has already been fed from the automatic speed change arithmetic circuit 40. The automatic speed change arithmetic circuit 40 calculates the difference between the engine speed set by the throttle lever 4 and the current engine speed, and outputs a speed change signal Sf to keep the engine speed from falling below the present current speed by a predetermined engine speed due to load variation. That is, ready-to-operate condition near the maximum horse-power point is created. The automatic speed change arithmetic circuit 40 comprises a subtracting point 41, a frequency-voltage converter 42, and a PID compensating circuit 43. To one input of the subtracting point 41 is fed a signal corresponding to the position of the throttle lever 4 from the potentiometer 23. The frequency-voltage converter 42 converts input pulse signals to a voltage signal corresponding responding to the number of pulses, feeding it to the other input of the subtracting point 41. The subtracting point 41 calculates the difference between the output signal of the potentiometer 23 and the output signal of the frequency-voltage converter 42, and outputs the resultant difference as a speed change signal Sf through the PID compensating element 43. The PID compensating element 43 is provided to prevent engine rotation and vehicle speed from becoming unstable during automatic speed change.
The subtracting point 51 subtracts the speed change signal Sf from the vehicle speed command signal Vs, and applies the result of subtraction to the servo drive circuit 50 via the switch 56. The servo drive circuit 50 is for controlling the direction and amount of discharge of the hydraulic pump of the transmission 10 and the suction amcunt of the hydraulic motor 12, and outputs the pump capacity change signal Sp and the motor capacity change signal Sm in the proportion preset according to the signal to be fed from the subtracting point 51. In addition, the servo drive circuit 50 determines the polarity of the pump capacity change signal Sp according to the polarity of the direction signal KFR. The pump capacity change signal Sp is fed to a coils 57a and 57b of a solenoid valve 57 which is for actuating the pump swash plate servo unit 14, while the motor capacity change signal Sm is fed to a coil 58a of a solenoid valve 58 which is for actuating the motor swash plate servo unit 15.
Accordingly, the pump swash plate servo unit 14 and the motor swash plate servo unit 15 control the slope angle of the swash plate based on the signals Sp and Sm, control the discharge amount of the hydraulic pump 11 and the suction amount of the hydraulic motor 12, and control the speed change of the transmission 10.
Now, the vehicle speed control arithmetic circuit 30 will be described in detail.
FIG. 3 shows a circuit diagram of an embodiment of the vehicle speed control arithmetic circuit 30. The potentiometer 21 outputs from voltage 0 to Vcc according to the position of the vehicle speed setting lever 2. Voltage 0 corresponds to the maximum backward speed set value, voltage Vcc to the maximum forward speed set value, and voltage 1/2Vcc to vehicle speed 0.
These voltage signals are fed to the negative input of a comparator C 1 and the positive input of a comparator C 2 respectively, and also fed to a contact S 1a of a switch S 1 via a resistor R 1 . To the positive input of the comparator C 1 and the negative input of the comparator C 2 , dead area setting voltages D b1 and D b2 for setting the dead area are fed. The setting voltage D b1 is higher than the voltage 1/2Vcc, and the setting voltage D b2 is lower than the voltage 1/2Vcc.
Accordingly, when the output voltage signal of the potentiometer 21 is within the range from the setting voltage D b1 to D b2 , both the comparators C 1 and C 2 become high level. As a result, no current flows to diodes D 1 and D 2 , and a movable contact piece S 1c of the switch S 1 contacts the contact S 1a .
When a voltage signal higher than the setting voltage D b1 is output from the potentiometer 21, the output of the comparator C 1 falls to the low level, and the movable contact piece S 1c of the switch S 1 contacts the contact S 1a . At this time, the above voltage signal is fed to the contact S 1a divided by resistors R 1 and R 2 . In the same manner, when a voltage signal lower than the setting voltage D b2 is output from the potentiometer 21, the output of the comparator C 2 falls to the low level, and the movable contact piece S 1c of the switch S 1 engages the contact S 1a . At this time, the difference (voltage) between the above voltage signal and the high level output voltage of the comparator C 1 is applied to the contact S 1a divided by the resistors R 1 and R 2 . That is, when the output voltage signal of the potentiometer 21 falls out of the dead area, the movable contact piece of the switch S 1 is transferred to the contact S 1a , while to the contact S 1a , a voltage of a given step-up value divided according to the resistance ratio of resistors R 1 and R 2 is applied. The above step-up value can be suitably set according to the resistance ratio of the resistors R 1 and R 2 . It is preferable that the step-up value is set so as to correspond to the minimum vehicle speed, that is, the minimum speed at which one can sense the speed.
By this means, whether the vehicle is running or in the stop state can be judged easily, and the dead area of high safety can be set. The circuit consisting of the above comparators C 1 and C 2 , resistors R 1 and R 2 , diodes D 1 and D 2 , and the switch S 1 corresponds to the dead area setting circuit 31 (FIG. 2) of the vehicle speed control arithmetic circuit 30.
On the other hand, outputs of the comparators C 1 and C 2 are fed to NAND circuits N 1 and N 2 which form flip-flop, respectively. As a result, when the output of the comparator C 1 falls to the low level, the NAND circuit N 2 outputs a high level signal to a line l 2 . When the output of the comparator C 2 falls to the low level, the NAND circuit N 2 outputs a low level signal to the line l 2 . The line l 2 is connected to switches S 2 and S 3 . When the line l 2 becomes high level, movable contact pieces S 2c and S 3c of the switches S 2 and S 3 engage contact S 2a and S 3a , respectively. When the line l 2 becomes low level, movable contact pieces S 2c and S 3c of the switches S 2 and S 3 engage contacts S 2b and S 3b respectively.
A comparator C 3 wherein the output of the switch S 1 is fed to its negative input and a signal corresponding to the present speed, i.e., a signal appearing in a line l 3 , is fed to the positive input is a comparator positive-feedbacked by a resistor R 3 , and outputs a deviation signal to diodes D 3 and D 4 so as to bring the signal in the line l 3 to coincide with the input voltage at a fixed width.
Accordingly, when the output voltage signal of the potentiometer 21 is in the forward and acceleration direction, the output of the comparator C 3 is fed to the negative input of an operational amplifier OP 1 through the diode D 4 , switch S 3 , and a resistor R 4 . When the above voltage signal is in the forward and deceleration direction, the output of the comparator C 3 is fed to the negative input of the operational amplifier OP 1 through the diode D 3 , switch S2, and a resistor R 5 . When the output voltage signal of the potentiometer 21 corresponds to the backward direction, the switches S 2 and S 3 are transferred by a low level signal appearing in the line l 2 , the output of the comparator C 3 is fed to the negative input of the operational amplifier OP 1 through the diode D 3 , switch S 2 , and resistor R 4 when the above voltage signal is acceleration, and to the negative input of the operational amplifier OP 1 through the diode D 4 switch S 3 , and resistor R 5 when the voltage signal is deceleration.
The operational amplifier OP 1 is a delay compensating integrator having the resistors R 4 and R 5 , and a capacitor BP 1 , and determines a delay time of the signal in the line 13 in the charge direction (acceleration direction) and the discharge direction (deceleration direction) based on the resistance values of the resistors R 4 and R 5 .
Accordingly, by suitably setting the resistance values of the resistors R 4 and R 5 an optimum delay time setting becomes possible so that proper acceleration feeling can be obtained at the acceleration time, and that deceleration shock does not occur at the deceleration time.
In either of the cases when the lever position of the speed setting lever 2 is transferred from forward to backward and when from backward to forward, a delay time in the acceleration direction is set. In this case, the signal in the line l 3 smoothly responds to from the signal corresponding to forward to the signal corresponding to backward or vice versa. This is due to the provision of the switch S 1 for setting the dead area before the comparator C 3 . The circuit consisting of the comparator C 3 , diodes D 3 and D 4 , switches S 2 and S 3 , resistors R 4 and R 5 , capacitor BP 1 , and operational amplifier OP 1 corresponds to the compensating circuit 32 (FIG. 2) of the vehicle speed control circuit 30.
The output voltage of an operational amplifier OP 2 is applied to the contact S 4a of the switch 4, the negative input of the operational amplifier OP 2 , and the positive input of the comparator C 4 . The operational amplifier OP 2 is an inverting amplifier, inverts the input voltage by the voltage 1/2Vcc, and applies the voltage thus inverted to the contact S 4b of the switch S 4 . The comparator C 4 is for identifying whether the input voltage is the forward area or the backward area. In the case of forward area, the comparator C 4 outputs a high level direction signal KFR, and brings the movable contact piece S 4c of the switch S 4 to engage the contact S 4a via a line l 4 . In the case of backward area, the comparator C 4 outputs a low level direction signal KFR, and brings the movable contact piece S 4c of the switch S 4 to engage with the contact S 4b via the line l 4 .
The circuit comprising the switch S 4 , operational amplifier OP 2 , and comparator C 4 corresponds to the absolute value circuit 33 and the discriminating circuit 35 (FIG. 2) of the vehicle speed control circuit 30, and the direction signal KFR is fed to the servo drive circuit 50.
The output voltage of the switch S 4 is applied to the positive input of an operational amplifier OP 3 . The operational amplifier OP 3 is a subtractor, and a brake signal associated with the depression (treading) of the brake pedal 3 is fed to the negative input.
The brake signal will now be described. The potentiometer 22 generates a voltage signal corresponding to the depression quantity (or depth) of the brake pedal 3, and applies to the positive input of a comparator C 5 , resistor R 6 , and diode D 5 . The comparator C 5 is designed to operate at the time of abrupt stop. When a voltage signal larger than the preset voltage Vb is generated at the potentiometer 22, the comparator C 5 instantly charges a capacitor BP 2 via a diode D 6 , and applies the input voltage to the positive input of the operational amplifier OP 4 . It is necessary to set the preset voltage Vb to a voltage sufficient for applying mechanical brake (mentioned later).
On the other hand, when a voltage signal smaller than the preset voltage Vb is generated at the potentiometer when the brake pedal 3 is depressed, the voltage signal is charged at the capacitor BP 2 via the resistor R 6 , and the charging voltage is fed to the positive input of the operational amplifier OP 4 .
When the brake pedal 3 is released, the electric charge given to the capacitor BP 2 is discharged by two systems of the resistor R 6 , and a resistor R 7 and the diode D 5 . That is, it is so designed that the delay time of the voltage signal (brake signal) appearing at the positive input of the operational amplifier OP 4 at the time of the depression of the brake pedal 3 differs from that at the time of release.
The operational amplifier OP 4 is a voltage follower circuit, and feeds the above brake signal fed to the positive input directly to the negative input of the operational amplifier OP 3 . The circuit comprising the comparator C 5 , diodes D 5 and D 6 , resistors R 6 and R 7 , capacitor BP 2 , and operational amplifier OP 4 corresponds to the brake signal compensating circuit 36 (FIG. 2) of the vehicle speed arithmetic circuit 30.
The operational amplifier OP 3 subtracts the brake signal from the voltage signal fed from the switch S 4 , and outputs the resultant signal as a vehicle speed command signal Vs.
Part of the vehicle speed command signal Vs is directed to the negative input of a comparator C 6 . The comparator C 6 is for actuating the mechanical brake 6. When the vehicle speed command signal has become smaller than the preset voltage V p , a high level voltage signal is output, thereby actuating the mechanical brake 6. The preset voltage Vp is to be a voltage slightly higher than the voltage signal (1/2Vcc) corresponding to the vehicle speed 0.
Consequently, when a voltage signal corresponding to the vehicle speed 0 is output from the switch S 4 without the depression of the brake pedal 3, the vehicle speed command signal Vs becomes voltage 1/2Vcc, and the mechanical brake 6 is actuated by the output of the comparator C 6 . That is, at the parking time, the mechanical brake 6 is actuated automatically. Of course, when the vehicle speed command signal Vs falls below voltage 1/2Vcc as a result of the depression of the brake pedal 3, the mechanical brake 6 is actuated. Furthermore, when a brake signal higher than the setting voltage Vb has been output from the potentiometer 22 as a result of the depression of the brake pedal 3, the mechanical brake 6 is actuated regardless of the voltage signal to be output from the switch S4.
In this embodiment, the vehicle speed control is designed to be accomplished by means of the signal generated as a result of the detection of the position of the vehicle speed setting lever, the position of the brake pedal, or the like, However, alterations and modifications may be made. For example, the above signal may be given by the operation of a radio control device. In addition, though this embodiment has been described in connection with the case when a single system of the transmission is used, similar construction may be made when two systems of the transmission are used. | In a vehicle speed control system, a vehicle speed command set corresponding to the position of a vehicle speed setting lever is fed into a dead area setting circuit in which the value of the vehicle speed command is changed to be not smaller than a preset minimum speed of the vehicle when it falls out of the dead area. Then the command is supplied into different delay compensating circuit depending on whether it is an acceleration command or a deceleration command. Further, the command outputted from the delay compensating circuit is subtracted by a brake signal generated by the operation of a brake pedal. The command thus subtracted causes a mechanical brake signal to generate when the speed of the vehicle is zero or minus. | 5 |
This application is the US national phase of international application PCT/NL2005/000120 filed Feb. 18, 2005 which designated the U.S. and claims priority to EP 04075539.9 filed Feb. 19, 2004, the entire content of each of which is hereby incorporated by reference.
BACKGROUND OF THE INVENTION
The present invention relates to the use of protein hydrolysate derived from keratin-containing material in the wet-end of a papermaking process, a process for preparing a paper product, and paper pulp and paper products comprising such a protein hydrolysate additive.
In the papermaking industry a wide variety of additives is applied to improve properties of the finished paper product. Such properties include, for instance, printability, wet/dry strength, softness and wetting properties. Generally, the amounts of additives to be used need to be carefully controlled because most of these additives are expensive chemicals.
BRIEF SUMMARY OF THE INVENTION
Object of the present invention is to provide a new class of cheap additives, which can attractively be used in the production of paper products.
Surprisingly, it has now been found that protein hydrolysate derived from keratin-containing material can attractively be used as a paper product additive with high retention.
Accordingly, the present invention relates to the use of a protein hydrolysate derived from keratin-containing material as an additive in the wet-end of a papermaking process.
The present invention enables the production of very high quality paper products in a very cost-effective manner. The paper products obtained in accordance with the present invention display excellent quality properties in terms of strength and volume per mass.
It will be appreciated that with the term wet-end is meant the stage of the papermaking process prior to the dry-end stage (the stage where the paper product to be made is dried).
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING(S)
FIG. 1 shows the Porosity of paper as compared to varying hydrolysate levels.
FIG. 2 shows the SCT index of paper as compared to varying hydrolysate levels.
FIG. 3 shows the Z-tensile of paper as compared to varying hydrolysate levels.
FIG. 4 shows the Breaking length of paper as compared to varying hydrolvsate levels.
FIG. 5 shows the Stretch at break of paper as compared to varying hydrolysate levels.
DETAILED DESCRIPTION OF THE INVENTION
The protein hydrolysate to be used in accordance with the present invention can be derived from a wide variety of keratin-containing materials. The keratin-containing materials can suitably be derived from mammals and/or birds. Suitable keratin-containing materials from which the protein hydrolysate can be derived include mammalian hair, animal hooves, claws, horns, and feathers. The protein hydrolysate is preferably derived from mammalian hair and/or feathers. More preferably, the protein hydrolysate is derived from mammalian hair, in particular from livestock, and more particularly from pigs and chicken feathers.
The protein hydrolysate to be used in accordance with the present invention can suitable be prepared by subjecting the keratin-containing material to an oxidation treatment in which the keratin-containing material is contacted with a solution, which comprises a bleaching agent. The solution to be used in the oxidation treatment has been made alkaline (above pH 7) or acidic (below pH 7). Preferably, the solution has been made alkaline by the addition of NaOH, KOH and/or NH 4 OH or acidic by the addition of one or more (organic) acid(s). A wide variety of (organic) acids can be used, including acetic acid and formic acid.
The pH value of the alkaline solution to be used in step (a) is preferably in the range of from 9-13, more preferably in the range of from 10-12. The pH value of the acidic solution is preferably in the range of from 3-7, more preferably in the range of from 4-6.
Suitable bleaching agents include organic and inorganic peroxides. Preferably, use is made of a bleaching agent selected from the group of hypohalides, perborates, percarbonates, organic peroxides, or hydrogen peroxide. More preferably, the bleaching agent comprises hydrogen peroxide. One single bleaching agent or a mixture of bleaching agents can suitably be applied in the alkaline or acidic solution. In the alkaline solution preferably inorganic peroxides are used, whereas in the acidic solution preferably organic peroxides are used. Suitably, the bleaching agent is used in an amount in the range of from 0.1% (w/w) to 40% (w/w), preferably in the range of from 0.3% (w/w) to 30% (w/w), based on total alkaline or acidic solution.
In the oxidation treatment the keratin-containing material can suitably be contacted with the alkaline or acidic solution over a period of time in the range of from 5 minutes to 16 hours, preferably in the range of from 15 minutes to 10 hours. The temperature to be applied in the oxidation treatment can suitably be in the range of from room temperature to 100° C., preferably in the range of from 30° C. to 80° C.
The keratin-containing material can be one type of keratin-containing material or it can be a mixture of different types of keratin-containing materials.
The keratin-containing material to be subjected to the oxidation treatment is preferably first subjected to a washing step in which soluble components, such as for instance blood, urine remnants and other animal components, are removed from the keratin-containing material before the keratin-containing material is subjected to the oxidation step. The protein hydrolysate obtained in the oxidation treatment and contained in the solution can subsequently be recovered by separating it from the remaining keratin-containing material. This can be established by means of known techniques. For this purpose use can, for instance, be made of a conventional filtering system. In this way a solution of the protein hydrolysate can be obtained. In order to recover the protein hydrolysate from the protein hydrolysate solution so obtained, the pH value of the solution can suitably be adjusted so as to allow the protein hydrolysate to precipitate, after which the protein hydrolysate precipitate can be recovered by methods known per se. The pH of the solution is preferably adjusted so as to be in the range of from 1 to 5, more preferably to be in the range of 2 to 4. The pH adjustment can be established by adding in a controlled manner, for instance by way of titration, an organic and/or inorganic acid to the solution. Suitable acids include hydrochloric acid, sulphuric acid, acetic and formic acid, and the like.
Suitably, the pH adjustment can be carried out over a period of time in the range of from 5 minutes to 10 hours, preferably in the range of from 20 minutes to 8 hours The temperature to be applied during the pH adjustment can suitably be in the range of from 15° C. to 100° C., preferably in the range of from 25° C. to 70° C.
Suitably, the protein hydrolysate precipitate obtained can be dissolved in a liquid medium to obtain a solution, which can be used as a paper product additive. Such a liquid medium suitably includes virgin and/or recycled cellulose fibres and/or known additives used in the wet-end of the paper process. Preferably, water or recycled water is used as the liquid medium. To the protein hydrolysate solution so obtained one or more other paper product additives can be added before the solution is used to produce a paper product. These other additives may contribute to different properties of the paper product to be obtained. The concentration of the protein hydrolysate will suitably be in the range of from 0.1% (w/w) to 50% (w/w), based on total fibre weight. Preferably, the concentration of the protein hydrolysate is in the range of from 0.3% (w/w) to 40% (w/w), based on total fibre weight.
Alternatively, the protein hydrolysate precipitate can as such be added to a solution containing one or more other additives to be used in the manufacturing of a paper product. In another suitable embodiment the protein hydrolysate precipitate is added directly to the paper pulp where after it is thoroughly mixed with other paper pulp components.
Preferably, the protein hydrolysate additive is used in the form of a solution.
The present invention also relates to a process for preparing a paper pulp comprising mixing in the wet-end a protein hydrolysate derived from keratin-containing material with virgin and/or recycled cellulose fibres, and recovering the paper pulp so obtained.
The present invention also relates to paper pulp obtainable by such a process. Suitably, such paper pulp comprises protein hydrolysate derived from keratin-containing material in an amount in the range of from of from 0.1 to 50 wt. %, based on total paper pulp. Preferably, such paper pulp comprises protein hydrolysate derived from keratin-containing material in an amount in the range of from 0.3 to 40 wt. %, based on total paper pulp.
The present invention further relates to a process for preparing a paper product comprising mixing the wet-end of a papermaking process a protein hydrolysate derived from keratin-containing material with virgin and/or recycled cellulose fibres, dewatering the mixture so obtained, pressing the dewatered material, drying the pressed material, and recovering the paper product so obtained.
Further, the present invention also relates to a paper product obtainable by such a process. Suitably, such paper product comprises protein hydrolysate derived from keratin-containing material in an amount in the range of from 0.1 to 50 wt. %, based on total paper product. Preferably, such paper product comprises protein hydrolysate derived from keratin-containing material in an amount in the range of from 0.3 to 40 wt. %, based on total paper product.
In the context of the present invention the term “paper product” is meant to include all sorts of papers, such as printing paper, tissue/hygiene, newspaper, office paper, specialties, but also materials such as cardboard, folding board, box board, undulated board, corrugated board, and 3D board and the like.
EXAMPLES
Preparation of Protein Hydrolysate.
To a mixture of 250 grams of hair was added 9 litres of water and subsequently the pH of the mixture was brought to a level suitable for bleaching. Then the temperature of the mixture was raised to 65-70° C. and 200 ml of a 30% (w/w) solution of hydrogen peroxide (pH 11) or 60 ml of a 32% (w/w) of peracetic acid (pH 5) was added. The mixture was then stirred for 16 hours after which the hydrolysate was isolated by lowering the pH of the reaction mixture to 3. Once the precipitate was formed it was collected through filtration and dried at 70° C. After drying, the obtained product may optionally be grinded into a powder.
Evaluation of the Protein Hydrolysate
The hydrolysate (0, 1, 5, 10, 15% (w/w)) was mixed with virgin cellulose fibres from Eucalyptus in such a way that for each mixture a constant weight of cellulose fibres was obtained. Also sheets were using only the virgin Eucalyptus cellulose fibres for comparison and evaluation results are depicted as 0% (w/w). The sheets were obtained by using a FRET (Formation and Retention Tester), using a vacuum of 0.5 bar. The sheets were dried at 100° C., using a Rapid Köthen drying cell. For each mixture three sheets were made.
From each mixture the paper properties were determined
Retention of the Protein Hydrolysate
Hand sheets were made on a Rapid Köthen (RK) sheet former as described above, and 360 mg of the keratine hydrolysate were added to the reservoir of the RK containing the fibre mixture (about 5 gram). Afterwards the filtrate (7 litres) was analysed according to the method of Bradfort on the protein content. It was measured that 0.722 mg/l was left in the filtrate. From this data it can be concluded that no less than 98.6% of the keratine hydrolysate was retained on the fibre.
Volume Per Mass (cm 3 /gram):
The volume per mass was calculated by dividing the thickness of the sheet by weight per m 2 . Table 1 gives the results of the different sheets
The volume per mass was reduced with increase of % protein hydrolysate. It seems that the protein hydrolysate was able to fill the pores formed by the cellulose fibre web.
TABLE 1 Volume per mass of sheets % Hydrolysate added (w/w) Volume per mass (cm 3 /g) 0 1.55 1 1.53 5 1.49 10 1.46 15 1.47
Porosity:
The effect of the addition of protein hydrolysate is depicted in FIG. 1 . With increase of the % added protein hydrolysate the porosity of the sheets decreased. The effect is clearly visible starting from 5% (w/w) added protein hydrolysate.
Short Compression Test:
The influence of protein hydrolysate as additive in cellulose pulp on the SCT index is depicted in FIG. 2 . The added protein hydrolysate has a positive influence on the short compression test index.
Z-Directional Tensile:
The influence of protein hydrolysate on the Z-directional tensile is depicted in FIG. 3 . FIG. 3 shows that increased addition of protein hydrolysate in cellulose fibre has a positive influence on the fibre interaction.
Tensile Index:
This parameter is measured to evaluate the force at break and gives an indication of the length of the paper needed before it breaks. FIG. 4 shows the results when part of the cellulose fibre is replaced by protein hydrolysate. There is a sharp increase on the length of break with increased weight percent of protein hydrolysate implying a stronger paper. This effect coincides with earlier observed improved fibre-fibre interaction.
Stretch at Break:
This parameter gives an indication of the amount of stretch of the paper sheet before it breaks. The results are depicted in FIG. 5 . The results fit well within the earlier results presented in FIGS. 3 and 4 . An increase in weight of protein hydrolysate also gives an increase in stretch at break. | A process for producing a protein hydrolysate derived from keratin containing material with an oxidative bleaching agent at an acidic pH and mixing the keratin hydrolysate as an additive to the wet-end of a papermaking process. The process achieves a paper with a lower porosity and greater breaking length. | 3 |
BACKGROUND OF THE INVENTION
The present invention relates to a method of uniformly applying liquid treating media to foraminous workpieces such as textile webs. The liquid treating media are to be foamed and applied to the workpiece in foamed condition.
A basic apparatus and method for this purpose have been disclosed in German Published Application DE-OS No. 2,523,062 which makes the advantages of applying the treating media in foamed state very clear. The known apparatus has a container above the workpiece, and the foam is deposited within this container, and is then squeezed through a wall of the container into the workpiece.
A problem with this approach is that the direct application of the foamed medium to the workpiece does not necessarily result in proper entry of the medium into the workpiece surface; depending upon the physical surface characteristics of the workpiece, surface differences from location to location, the chemical condition of the workpiece surface and the uniformity of any chemical application (or even the condition within the confines of the workpiece), the foam bubbles will burst at different rates of speed so that different quantities of released treating liquid are available for different surface areas. In other words: application of the foam to the workpiece and squeezing of the foam into the workpiece through a side edge of the application chamber does not assure uniform entry of the foam into the workpiece.
On the other hand, it is desired that foam carrying e.g. liquid ink particles or other substances transport liquid only in minimum quantities and that this liquid be completely yielded up to (absorbed by) the workpiece.
OBJECTS AND SUMMARY OF THE INVENTION
An object of the invention is to provide an improved method of treating a foraminous workpiece such as a textile web with foamed treating medium.
Another object is to ensure that the foam is deeply transported into the structure of the workpiece and that the surface of the workpiece is also provided with released (by the foam) liquid treating medium.
A concomitant object of the invention is to deposit the foam over a very small surface area of the workpiece at any one time.
In the method according to the invention the foamed treating medium is applied to the workpiece within a circumambiently restricted area such as four-sidedly delimited area, whereupon it is first drawn into the workpiece by suction and subsequently pressed in by squeezing. An advantage of this method is that the liquid carried by the sucked-in foam reaches deep into the workpiece (possibly as deep as the substrate) whereas the surface of the workpiece receives liquid foam bubbles which burst when squeezed into the surface. This eliminates the soaked "grey-veil" effect, which is especially important in the case of napped fabrics, for example carpeting or the like.
It is well known that napped textiles come in various degrees of hardness. According to the invention it has now been found that especially in the harder qualities of such textiles the surface structure of the workpiece acts in effect as a sieve or screen. This means that the workpiece surface structure destroys the foam bubbles, causing them to release their contained liquid; the application of this liquid is completely uniform over the entire area of application. The quantity of foam supplied per unit time is adjustable, and the vacuum used to draw it into the workpiece is also variable. This means that the quantity of liquid entering the workpiece per unit time can be maintained within a desired tolerance range of 1 to 5% in relationship to the liquid which it is desired to apply per surface area. This very exact result cannot be achieved with the prior art, since the angle of the side edge of the prior-art box is not variable; even if a doctor blade were used at this point, this could not change the quantity of liquid entering the workpiece.
An apparatus for carrying out the invention comprises means defining above the workpiece a space or container which is closed at four sides, one side of which is an applicator device such as a squeegee. Below the plane of passage of the workpiece there is arranged a suction device; as considered in the direction of workpiece movement, the applicator device is arranged downstream of the suction device.
A supply device may be provided which feeds the foamed treating medium into the container, one wall of which is wholly or in part constituted by the applicator device. The suction device may be a suction box with a suction slot. The applicator device downstream of the suction device may be a roller squeegee which may or may not be separately driven. The suction of the suction device is variable and the suction device may be located immediately upstream of the roller squeegee. Both the applicator device and the suction device preferably extend all the way across the working width of the apparatus.
When the foam is applied to the workpiece it is destroyed (the bubbles burst) and a minimum but adequate amount of released treating liquid is then available uniformly over the entire surface area of the workpiece, since such uniformity is assured by the applied suction which also determines the amount of liquid that is allowed to remain at the surface of the workpiece (instead of being drawn in).
A further advantage of using relatively low-grade adjustable suction resides in the fact that air is withdrawn from the interstices of the foraminous workpiece, thus allowing the liquid released by bursting of the foam bubbles to enter the workpiece much more easily. Also, mechanical resistance at the workpiece surface is thereby eliminated.
On the other hand, the additional mechanical squeegeeing of the foam, preferably but not necessarily by a roller squeegee, at a location downstream of the suction application, has the advantage that any not already burst bubbles are now definitely burst and made to release their liquid; further, it removes residual foam and liquid from the workpiece surface.
The invention is particularly suited for continuous operation. However, discontinuous operation is certainly possible. It would then only be necessary to make the suction device (and preferably the squeegee) movable backwards and forwards in direction of workpiece movement.
The invention will hereafter be described with reference to exemplary embodiments. These, however, are merely for the purpose of explanation.
BRIEF DESCRIPTION OF THE DRAWING
FIG. 1 is a diagrammatic side elevational view of one embodiment of an apparatus for the practice of the novel method;
FIG. 2 is a similar view, but of a different apparatus for discontinuous operation;
FIG. 3 is a view analogous to that of FIG. 1, but illustrating a further apparatus; and
FIG. 4 is a diagrammatic side elevational view, illustrating an apparatus for the practice of the method and a foam generator therefor.
DESCRIPTION OF PREFERRED EMBODIMENTS
Common to the apparatus of all embodiments is that they serve for the uniform application of liquid but foamed treating media to any kind of textile workpieces, especially webs. The invention is especially useful in napped workpieces, such as carpeting or the like, but is not limited thereto. The method will be explained in conjunction with the operation of the apparatus.
In FIG. 1, reference numeral 2 identifies the foam supply device which may be a hose, pipe or duct provided with outlets 20 which are uniformly spaced over the width of the workpiece. The foam generator will be described with reference to FIG. 4.
The workpiece 1 can--and, in view of the application of suction, as a rule will--rest on an air-permeable printing blanket 3. This may be endless, as shown in FIG. 2. However, instead of a printing blanket the workpiece may pass over a known-per-se screen drum in which the suction device 4 is then arranged. In the embodiments of FIGS. 1, 2 and 3 (in all embodiments like reference numerals identify like elements) the suction device is a suction box which extends over the entire working width of the apparatus and is provided with a suction slot 40. If a screen drum is used (not shown) the suction device will be of segmental shape.
FIG. 1 shows that atop the textile workpiece 1 there is arranged a space--e.g. the interior of a container 5--bounded on four sides but open to the workpiece. The foamed medium is deposited in this space by the device 2. In place of a container 5, sidewalls 50 could be used which could be adjustable relative to one another, and a front wall 55 be provided at the side at which the workpiece is incoming (as considered in the direction of workpiece movement).
Arranged below the container 5 or its substitute is the suction device 4 with its suction slot 40. Device 4 is connected with vacuum pump 41. The suction regulation is effected via a valve 141 or the like. Pump 41 can be connected with the suction device 4 via a hose (FIG. 4) or a stationary pipe 42'. What type of known-per-se vacuum pump or producer is used, is immaterial. Suction device 4 should be adjustable in its position (in the movement direction of the workpiece), but should preferably be fixed once it is set to a selected spot.
The rear wall 52 (as considered in the direction of workpiece movement) is partly formed by the applicator device 6. In FIG. 1 this is a doctor blade whose angle in relation to the movement of the workpiece is adjustable. The workpiece 1 on the printing blanket thus passes under the container 5 and over the suction device 4, whereupon it travels under the mechanical doctor blade so that the foam, after being sucked into the workpiece, is also pressed into the surface layer of the same. The wall 52 above device 6 prevents overflowing of the foam.
FIG. 2 shows a somewhat similar apparatus with an applicator device 6 which this time is constructed as a roller squeegee. The front wall 55 is supported on a traverse member 51 which can be secured in the machine frame at opposite sides of the apparatus; it is adjustable in the indicated arrow directions and can be arrested at any desired distance from the applicator device 6. Wall 55 may be specially profiled to form a channel 53 through which the foam can most expeditiously flow downwards.
Rear wall 52 is supported via a sealing strip 152 on the surface of the roller squeegee 6; the seal is adjustable to keep it tight. This wall, also, is supported on a traverse member which can be secured to the left and right of the workpiece in the machine frame. Suction device 4 is similar to the one in FIG. 1.
The embodiment of FIG. 3 has another roller squeegee as the applicator device 6; but it has a stationary container 5 and therebelow a suction device 4.
The Figures all show that the printing blanket 3 can be guided over rollers 30, 31. Evidently, it is both air and liquid-permeable. The rollers for it can be driven continuously or discontinuously; the former is generally preferred.
The low-grade vacuum, whose strength can be controlled, removes air from the workpiece so that a uniform, resistance-free entry of the liquid into the workpiece is obtained.
All embodiments show a napped workpiece, because the invention is particularly advantageous for such material. The suction device may also be an area-spanning box.
Due to the adjustability of the portion of the suction device 4 relative to applicator device 6 (e.g. roller squeegee) the effect of the suction device can be further selected. If it is desired to first remove air from the workpiece, the suction slot is located further away from device 6. If an effect is to be obtained on the already mechanically pressurized foam, the suction slot 40 is located close to the applicator device 6 (e.g. roller squeegee) under the wedge 60 defined by the applicator device 6 and the web 1 (see FIGS. 2 and 3).
FIG. 4, finally, shows one embodiment of a foam generator for the apparatus in FIGS. 1-4. The liquid treating agent (of any kind that can be foamed) is contained in a reservoir 90. Compressed air is supplied from a compressor 91 or analogous device. The two are connected with a mixing head 94 via conduits 190, 191 in which quantity-measuring devices (known-per-se) 290 and 291 are installed. Control valves are also provided; only the valve 92 for conduit 191 is shown.
Liquid is pumped from reservoir 90 via a pump 93 which is driven by a motor 193 via a transmission 293. Thus, both liquid and compressed air enter the mixing head 94 which has a mixing chamber 194 containing glass beads, granulate or the like to aid in the foam formation. The compressed air is admitted into an annular space 294 surrounding chamber 194 and enters the same from below via appropriate openings. The thus created foam is then passed via a conduit, pipe, hose or the like 95 in a precisely set mixing ratio to the device 2, and from there onto the workpiece. A main shut-off valve 96 is interposed in air line 191.
The stream of foam flowing toward the point of application should be continuous and the rate of feeding the foam should match the consumption.
The squeegee device and the suction device can be built as a compact unit. The device 4 can be built so that the suction device and the squeegee device work upon the opposite sides of the same portion of the substrate. | Liquid treating medium is uniformly applied to a textile workpiece by foaming it, depositing the foam in a confined space atop the workpiece, applying suction to the workpiece from below and thereafter mechanically pressing additional foam into the surface layer of the workpiece. | 3 |
FIELD OF THE INVENTION
The invention relates to a tomographic synthetic aperture radar (SAR) method operating with an airborne or spaceborne radar sensor for three-dimensional object imaging in which a true three-dimensional image is obtained by coherent combination of a plurality of SAR sensor images obtained at differing viewing angles. The backscatter contributions of volume targets are separated in elevation and can be analyzed each independent of the other.
BACKGROUND
Imaging radar methods operate with an active radar sensor which, by means of radiating and receiving electromagnetic waves in the microwave range, generates a reflectivity map of the illuminated area. In recent years synthetic aperture radar (SAR) has attained major significance in remote sensing due to the high resolution and rich information content of SAR images. In addition to traditional applications in geography and in topographical and thematic mapping, SAR sensors also find application nowadays in many other fields such as e.g. in oceanography, agriculture and forestry, urban planning, ecology as well as in the forecasting and evaluating natural disasters.
One salient property of SAR methods materializes from the propagation properties of microwaves. Due to their long wavelength they are able to penetrate vegetation and even the ground down to a certain depth, depending on the wavelength as well as on the dielectric constant and density of the object concerned. Radiation of shorter wavelength, such as X band radiation, exhibits a strong attenuation and is backscattered primarily by the upper portions of the vegetation, whereas radiation of longer wavelength, such as L and P band typically penetrates deeper into the vegetation cover and ground. Backscatter thus contains contributions of all layers attained by the radiation.
One main problem in analyzing conventional SAR images of longer wavelengths is the layover of several backscatter contributions. Although a certain backscatter contribution of interest is buried in the data, this is often inaccessible since it is only the backscatter as a whole that can be sensed. Another problem is establishing the precise vertical position of the backscatter location, which is unknown since SAR geometry as a whole exhibits symmetry in elevation. This is why the elevation angle or the topographical elevation of the backscatter cannot be resolved by a conventional SAR method.
One known imaging SAR method is the so-called SAR interferometry (INSAR) as described in the paper R. Bamler and P. Hartl: “Synthetic Aperture Radar Interferometry”, Inverse Problems, Volume. 14, pages R1-R54, 1998, which is understood to be a technique by which the phase difference between two SAR images, taken at slightly different positions, is evaluated. This phase difference is a function of the elevation angle involved and thus of the topography of the terrain concerned. This permits generating highly accurate digital elevation models (DEMs) from INSAR images in which the elevation of a mean scatter center is decisive for each pixel of the image.
Making use of various wavelengths or polarizations opens up the additional possibility of determining the elevation of a plurality of scatter centers characteristic for each wavelength or polarization concerned; this can be used in determining the thickness of vegetation layers. By inverting simple scatter models, further physical parameters, such as e.g. the attenuation constant, can be additionally determined.
SAR interferometry (INSAR) has, however, more particularly the disadvantage that it is exclusively the elevation of a mean scatter center that can be measured, i.e. this method fails to achieve true three-dimensional imaging. Thus where volume targets are concerned, layover of the various scatter centers continues to be a problem. This is why the INSAR method is unsuitable for a detailed analysis of volume targets. On top of this, INSAR measurements fail to be completely unambiguous, and a further processing step is needed, namely phase unwrapping, to eliminate these ambiguities.
Model-based approaches on the basis of polarimetric or multifrequent interferograms are restricted, in principle, to a few simple parameters in analyzing volume targets. Their scope of application is thus very limited. Apart from this, they greatly depend on the scatter model employed and are a total failure when the assumptions made fail to apply.
Another technique for analyzing three-dimensional objects is multi-pass tomography, as known from the paper by A. Reigber and A. Moreira: “First Demonstration of Airborne SAR Tomography using Multibaseline L-band Data”, IEEE Trans. on Geoscience and Remote Sensing, Volume 38, No. 5, pages 2142-2152, September 2000. In this technique, a true three-dimensional image is obtained by coherent combination of a large number of SAR images at various viewing angles. The backscatter contributions of volume targets are separated in the elevation and can thus be analyzed each independently of the other. It is also possible to combine this technique with polarimetry to thus permit attaining indications not only as to the three-dimensional distribution of the scattering processes but also as to the type of the scattering process concerned in each case.
The main problem in multi-pass tomography is the extremely high experimental complications involved. Only with a large number of parallel passes (>10) good resolution coupled with a good information content, is attainable. This necessitates lengthy flight times for a relatively small imaged portion. Since the relative distances between the passes need to be known to within a millimeter for data processing, the multi-pass technique makes high demands on the positioning of the sensor. These requirements have hitherto been satisfied only to an inadequate extent. In conclusion, the unavoidable lack of uniformity in the distribution of the passes greatly restricts the quality of imaging. This is why multi-pass tomography is to be appreciated only as functional verification of airborne SAR tomography.
Known further from U.S. Pat. No. 5,463,397 A is a SAR interferometry system as a combination of multi-pass interferometry with successive dual-antenna SAR interferometry to obtain elevation maps with an accuracy unobtainable by either method alone. However, here too, the disadvantages of the multi-pass tomography as described above occur.
Separating the backscatter contributions in accordance with the elevation can also be achieved by the radar pulses emitted vertically downwards, as described in the paper by M. Hallikainen, J. Hyyppa, J. Haapanen, T. Tares, P. Ahola, J. Pulliainen, M. Toikka: “A helicopter-borne eight-channel ranging scatterometer for remote sensing—Part 1: System Description”, IEEE Trans. On Geoscience and Remote Sensing, Volume. 31, No. 1, pages 161-169, 1993. Here, unlike in the two methods as described above, resolving elevation is achieved by delay measurement of the radar.
Although a good elevation resolution is achievable by downwards emitted radar pulses, the three-dimensional resolution is poor. The swath of such an image needs to remain narrow to permit a near vertical angle of incidence, thus making large-area imaging impossible.
It is very similar to this that light detection and ranging (Lidar) sensors offer the basic possibility of three-dimensional object analysis. Here, instead of microwave pulses, short laser pulses are emitted vertically downwards, precise delay measurement in turn making elevation resolution possible. Thus, both methods enable profiles along the pass of the sensor to be determined. Similar as for radar pulses emitted vertically downwards, Lidar systems too, permit achieving only a narrow swath, since otherwise a fringing angle of incidence would not permit penetration of the laser pulses down to the ground. However, even with vertical incidence a Lidar system depends on small clearances in a forest in being able to penetrate to the ground and is thus greatly dependent on the type of forest concerned. Clouding too, prevents application of the Lidar system. In general, Lidar is only suitable for measuring the height of vegetation; it cannot be used for three-dimensional volume analysis.
SUMMARY OF THE INVENTION
The invention is based on an airborne or spaceborne SAR configuration which is able to perform a three-dimensional imaging of volume scatterers. This involves, for instance, three-dimensional analysis of the backscatter contribution of vegetation layers, determining their layer thickness and biomass, as well as correcting for falsification in the backscatter of the ground located underneath caused by vegetation. Being able to determine the topographic elevation from the elevation angle of the backscatter, precise and free of ambiguities, would also open up possible applications in three-dimensional imaging and mapping of buildings, urban areas and mountainous terrain.
In accordance with the invention relating to a tomographic radar method of the aforementioned kind, this object is achieved by the various viewing directions being formed by a set of SAR antennas each working independently of the other in simultaneous operation. Unlike the known multi-pass tomography, as explained above, in which the various viewing angles are achieved by repeated passes in parallel, in the method in accordance with the invention a set of independent SAR antennas is operated simultaneous instead. The method as proposed by the invention eliminates the disadvantages experienced in multi-pass tomography.
The method in accordance with the invention offers a number of advantages. For one thing, it now makes it possible to unambiguously determine the origin of all scatter contributions, irrespective of assumptions as to the imaged objects. The method in accordance with the invention permits true three-dimensional imaging of the site being remotely sensed. A single pass is all that is needed for complete data acquisition in thus greatly reducing the operational expense whilst avoiding unequal distribution of the passes and the attendant poor imaging quality. Likewise avoided is a temporal decorrelation during data acquisition.
Advantageous further embodiments and aspects of the invention read from the sub-claims relating back to claim 1 either directly or indirectly.
In the case of airborne radar sensors the various viewing directions are formed by individual SAR antenna elements of an antenna array, fixedly secured to the aircraft each relative to the other in a fixed physical relationship in simultaneous operation. Fixedly securing the antenna elements to the aircraft reduces the requirements on the absolute position of the sensor to a reasonable degree. The relative spacing vectors between the antenna elements can be exactly defined in designing the sensor.
The radar sensor in the method in accordance with the invention is operated as a rule side-looking.
One variant of the method in accordance with the invention is to operate such a sensor forwards-looking instead of side-looking to thus achieve high elevation resolution even with a small antenna array. The long synthetic aperture materializing from the forwards movement of the sensor results in a very high elevational resolution in the forwards-looking direction. A high range resolution results from the delay sensing of the radar itself. In the direction perpendicular to the movement direction of the sensor in the horizontal plane, the resolution is related to the length of the real aperture of the antenna array perpendicular to the direction of flight.
Another variant of the method in accordance with the invention is downwards-looking operation. In this case, the long synthetic aperture in the direction of flight produces a high azimuthal resolution; the elevational resolution materializes from the delay sensing of the radar. Perpendicular to the direction of movement of the sensor higher resolution is obtained by the real aperture of the antenna array in this direction.
Where spaceborne sensors are concerned, a fixedly secured antenna array cannot be put to use since the sizes for such an antenna array are of the order of several kilometers. Instead of a fixedly secured antenna array, this can only be achieved by an adequate arrangement of physically separated sensors. Where satellite-borne radar sensors are concerned, the various viewing directions are thus formed to advantage by simultaneous operation of the individual SAR antennas of receivers on physically separated satellites of a cluster thereof moving in unison, transmission being made by one satellite of the cluster.
One variant of the method in accordance with the invention is the extension of the cartwheel concept of D. Massonet (WO 99/58997) to a larger number of satellites for implementing three-dimensional object imaging. By distributing the receiving satellites sufficiently expanded in space high-quality imaging is achievable also over great distances.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be detailed by way of example embodiments with reference to the drawings in which
FIG. 1 is an illustration showing the imaging geometry for three-dimensional object imaging in a side view, an antenna array observing a volume target from various viewing angles,
FIG. 2 is an illustration showing a simplified tomographic imaging geometry,
FIG. 3 is an illustration showing in two plots ( FIG. 3 a and FIG. 3 b ) the simulated pulse responses of a side-looking tomographic radar sensor,
FIG. 4 is an illustration showing in two plots ( FIG. 4 a and FIG. 4 b ) the simulated pulse responses of a forwards-looking tomographic radar sensor,
FIG. 5 is an illustration showing in two plots ( FIG. 5 a and FIG. 5 b ) the simulated pulse responses of a downwards-looking tomographic radar sensor,
FIG. 6 is an illustration showing the imaging geometry in principle of an airborne forwards-looking tomographic radar sensor,
FIG. 7 is an illustration showing the imaging geometry of an airborne forwards-looking tomographic radar sensor illustrating the aperture lengths,
FIG. 8 is an extension of the cartwheel concept working in accordance with the method in accordance with the invention for three-dimensional object imaging from spaceborne sensors,
FIG. 9 is another extension of the cartwheel concept working in accordance with the method in accordance with the invention for three-dimensional object imaging from spaceborne sensors, and
FIG. 10 is yet another extension of the cartwheel concept working in accordance with the method in accordance with the invention for three-dimensional object imaging from spaceborne sensors, achieving a uniform distribution of the various viewing angles.
DETAILED DESCRIPTION
Referring now to FIG. 1 there is illustrated in a Cartesian x-y-z-system of coordinates the basic geometry of a radar sensor in a side view for three-dimensional object imaging. The movement of the sensors is to be imagined parallel along the x axis. The various independent antenna elements of an antenna array are arranged so that each thereof (paths 1,2 . . . N-1, N of the antenna elements) views the scene and thus the volume targets V at a different angle.
Referring now to FIG. 2 there is illustrated a simplified geometry in which an array of antenna elements has the aperture length L and the center-spacing of the antenna elements is d and the mean angle of incidence is 0°, i.e. the n axis as shown in FIG. 1 is parallel to the z direction. In this geometry the spacing between a scatter at the elevation n 0 and the antenna element at the position z is
r ( z , n 0 ) = 2 r 0 2 + ( z - n 0 ) 2 ≈ 2 r 0 + ( z - n 0 ) 2 r 0 ( 1 )
The signal s r (z, n 0 ) received by this antenna element can thus be modeled as follows:
s r ( z , n 0 ) = a ( n 0 ) exp ( - ik r 0 ( z - n 0 ) 2 ) , ( 2 )
where k=2π/λ is the wave number of the emitted waves and a(n 0 ) is the complex reflectivity at elevation n 0 . An approach similar to that of the SPECAN method is useful for processing. When this signal is multiplied by a deramping function u(z)
u ( z ) = exp ( + ik r 0 z 2 ) , ( 3 )
then a signal materializes whose wave number in the z direction is no longer a function of z but merely of the elevation of the scatter n 0 :
s d ( z , n 0 ) = a ( n 0 ) exp ( - ik r 0 ( n 0 2 - 2 zn 0 ) ) . ( 4 )
so that the spectral k z range is proportional to the spatial n range in conjunction with the relation k z =2kn 0 /r 0 . Thus, by a Fourier transformation in the z direction the imaging result v(n, n 0 ) is:
v ( n , n 0 ) = FT z ( s d ( z , n 0 ) ) = a ( n 0 ) L exp ( - ikn 0 2 r 0 ) sin c ( kL r 0 ( n 0 - n ) ) . ( 5 )
Resolving this imaging result in the n direction is attained from the first zero positions of the “Sinus Cardinalis” function and is
δ n = λ r 0 2 L . ( 6 )
For instance, a system in the L band at an altitude of 500 m and a total extent of the antenna array of 30 m would produce a resolution of roughly 3 m.
Also to be taken into account is the center-spacing d of the individual antenna elements. So that the signal spectrum generated by a volume of elevation H is sufficiently sampled, the requirement
d ≤ λ r 0 2 H ( 7 )
need to be satisfied, otherwise serious ambiguities materialize within the volume analyzed.
The resolutions in range and along the pass are identical to those of a conventional SAR sensor and are cτ/2 and L az /2 respectively where c is the speed of light, τthe pulse duration and L az is the length of the antenna in the direction of flight.
Referring now to FIG. 3 a and FIG. 3 b there are illustrated in the x-y and y-z plots respectively the simulated pulse responses of a side-looking tomographic radar sensor working in accordance with the invention. The system parameters for this simulation are: L band, 150 MHz bandwidth, 1000 m altitude, length of the antenna array L γ =25 m with 30 elements, azimuthal synthetic aperture 500 m and squint angle χ=0°.
Referring now to FIG. 6 and FIG. 7 there is illustrated the imaging geometry in principle of an airborne forwards-looking radar sensor working by a method in accordance with the invention. Deriving the elevational resolution is analogous to that as described above. In this case, however, it is not the extent of the antenna array but the projection of the synthetic aperture in the direction of flight on the direction perpendicular to the viewing direction that decides focusing, as is evident from FIG. 7 . Its length L n depends on the off Nadir angle θ and L n =L sa cos(θ). With the same quadratic approach as in equation (1) and in using L n =λcos (θ)/L we have
δ n = λ r 0 2 L n = L 2 cos ϑ , ( 8 )
where L is the real aperture of the antenna in the direction of flight. Similar to the situation with conventional SAR in the direction of flight, this resolution no longer depends on the range. This is why the resolutions achievable are comparable to conventional azimuthal resolutions and may attain one meter or less with no problem. The problem of sampling lacking uniformity and undersampling as involved in multi-pass tomography can be ignored in this case, since strong oversampling of the data is achievable also for large volume thickness due to a more or less constant flight velocity and a sufficiently high pulse repetition frequency.
Available in the y direction is only the real length L γ as formed by the antenna array. The resolution in this direction can be derived the same as above. Since the resolution materializes from a real aperture, it is a function of the range and attains its maximum value in the direct forwards direction (squint angle χ=90°). On the sides, with sinking squint, the resolution is also diminished since the effective aperture is reduced:
δ y = λ r 0 2 L y cos ( χ ) . ( 9 )
Due to the limited extent of the antenna array and the range dependency of the resolution, δ γ is relatively slight for usual system parameters. Despite this, an acceptable resolution is achievable with a relatively low altitude and small size of the antenna array. For example, an antenna array having an overall length of 5 m exhibits in a range of 1,000 m a resolution of 25 m.
Referring now to FIG. 4 a and FIG. 4 b there is illustrated in an x-y plot and x-z plot respectively the simulated pulse responses of a forwards-looking tomographic radar sensor working in accordance with the invention. The system parameters for this simulation are: L band, 150 MHz bandwidth, 1,000 m altitude, length of antenna array L γ =10 m with 20 elements, azimuthal synthetic aperture 500 m and a squint angle χ=90°.
The results for the downwards-looking variant are similar, except that the elevation resolution in this case is dictated purely by the accuracy of the delay measurement. The resolution in the direction of flight corresponds to that of a conventional SAR sensor; perpendicular to the direction of flight, equation (9) again applies, where χ represents the side-looking angle. Simulated pulse responses are shown in FIG. 3 c.
Referring now to FIGS. 5 a and 5 b there is illustrated in an x-y plot and x-z plot respectively the simulated pulse responses of a downwards-looking tomographic radar sensor working in accordance with the invention. The system parameters for this simulation are: L band, 150 MHz bandwidth, 1,000 m altitude, length of antenna array L γ =10 m with 20 elements, azimuthal synthetic aperture 500 m and a squint angle χ=90°.
Referring now to FIG. 8 and FIG. 9 there are illustrated two different possibilities for an extension of the spaceborne cartwheel concept working by the method in accordance with the invention. In this concept a transmitting master satellite MS is followed by a plurality of receiving satellites ES which receive the signals backscattered by the object OB following irradiation by the master satellite MS. Suitably setting the orbit OR, in which the satellites ES and MS achieve stable motion, the receiving satellites in FIG. 8 and FIG. 9 will form an appropriate configuration flying equispaced on an ellipse E 0 behind or ahead of the master satellite MS. Arranging a larger number of receiving satellites ES in one or more cartwheels located parallel to each other in a single plane following the master satellite MS permits achieving multiple viewing angles on the object. In the example aspect as shown in FIG. 9 the receiving satellites move on two cartwheel ellipses E 1 and E 2 following the master satellite MS.
Referring now to FIG. 10 there is illustrated another possibility of extending the spaceborne cartwheel concept working by the method in accordance with the invention. In this case, only a single receiving satellite ES orbits on each of several cartwheel ellipses oriented parallel to each other in a single plane. All of the receiving satellites ES are located on a common focus beam of all ellipses E 0 and follow the master satellite on the orbit OR.
A cartwheel system works side-looking and thus the elevational resolution is given by equation (6). In this case, the aperture length L is the diameter of the complete arrangement. For example, a cartwheel system in the L band at an altitude of 500 km would require a diameter of approx. 30 km for an elevational resolution of 3 m, necessitating in an arrangement as shown in FIG. 10 a total of 10 satellites to image a volume with a thickness of 30 m free of ambiguities. | By means of tomograhic radar technique consisting of a coherent combination of large numbers of synthetic aperture radar images acquired by several air or space SAR systems having different look angles, a real three-dimensional imaging of volume scatterers is achieved. This allows the separation of the backscattered signal of volume scatterers in the height direction which can be further evaluated independently. The invention can be put to use in the three-dimensional analysis of vegetation layers and ground strata, but also for imaging and mapping of buildings, urban areas and mountainous terrain. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is the U.S. National Phase of PCT Appln. No. PCT/EP2015/077096 filed Nov. 19, 2015, which claims priority to German Application No. 10 2014 225 460.4 filed Dec. 10, 2014, the disclosures of which are incorporated in their entirety by reference herein.
BACKGROUND OF THE INVENTION
1. Field of the Invention
[0002] The invention relates to a process for the direct synthesis of methylchlorosilanes by reaction of chloromethane with a contact composition containing silicon, copper catalyst and promoter.
2. Description of the Related Art
[0003] In the Müller-Rochow direct synthesis, chloromethane is reacted with silicon in the presence of a copper catalyst and suitable promoters to form methylchlorosilanes, with not only a very high productivity (amount of silane formed per unit time and reaction volume) and a very high selectivity, based on the target product dimethyldichlorosilane, but also a very high silicon utilization combined with safe and at the same time flexible operation of the overall plant being demanded. Dimethyldichlorosilane is required, for example, for the preparation of linear polysiloxanes.
[0004] The direct synthesis can be carried out batchwise or continuously. The continuous direct synthesis is carried out in fluidized-bed reactors in which chloromethane is used simultaneously as a fluidizing medium and a reactant. The silicon required is milled beforehand to give a powder having a particle size of up to 700 μm and mixed with copper catalysts and promoters to form the contact composition; this is referred to as fresh contact composition (=contact composition 1). Contact composition 1 is subsequently introduced into the fluidized-bed reactor and reacted at a temperature in the range of 260-350° C. This forms an active contact composition (=contact composition 2), i.e. contact composition containing active sites. (Lewis and Rethwish, Catalyzed direct reaction of silicon, Stud. Org. Chem. 1993, 49, 107). Methylchlorosilanes are formed in an exothermic reaction at these active sites.
[0005] Unreacted chloromethane, the gaseous methylchlorosilanes and contact composition constituents leave the reactor. To ensure a high silicon utilization, these constituents can be recirculated in their entirety or in part back to the reactor. For example, the coarser part of the entrained contact composition particles can be separated off from the gas stream by means of one or more cyclones and optionally be recirculated via intermediate collection vessels back into the reactor. Since activated constituents of the contact composition are present here, these are a part of the contact composition 2.
[0006] The very finely particulate, entrained particles (=contact composition 3), which still comprise high proportions of copper and secondary elements in addition to silicon, likewise have to be separated off from the gas stream. This can, for example, be effected by gas filtration and/or one or more subsequent cyclones. This procedure with discharge of reacted particles can make a continuous process possible and ensure a high silicon utilization.
[0007] As an alternative, the entire entrained solids stream can be separated off and discharged from the system continually or only at particular intervals.
[0008] U.S. Pat. No. 4,281,149, FIG. 1, depicts by way of example such a system consisting of reactor, main cyclone with recirculation and after-cyclone with dust collection container. The crude silane is subsequently separated off from unreacted chloromethane and passed to a distillation. Purified, unreacted chloromethane can be fed back into the reactor.
[0009] The collected contact composition 3 has to be discharged since various secondary elements and proportions of slag which are introduced with the silicon have accumulated in this product stream, and if it were recirculated in its entirety into the reactor, the selectivity would be greatly reduced by catalytic effects of these impurities. Likewise, an accumulation of inert secondary elements which would reduce the on stream time of the reactor would occur. The ratio of contact composition 1 to contact composition 2 can vary greatly, in particular as a result of the above-described recirculation. Contact composition 2 is an active contact composition and already comprises a sufficient amount of copper and promoters. Contact composition 2 is able to react with chloromethane at relatively low temperatures and to produce silanes with high productivity and dimethyldichlorosilane selectivity. When contact composition 1 and contact composition 2 are mixed in the reactor, an unfavorable distribution of catalyst and promoters can occur since catalyst constituents also bind to activated particles and thus, for example, unnecessarily increase the consumption of catalyst or bring about an incorrect distribution of the active constituents.
[0010] To counter these disadvantages, the prior art discloses thermal pretreatment of the fresh contact composition. US 2003/0220514 describes a process in which silicon is thermally treated together with copper oxide and/or copper chloride at temperatures of 250-350° C. SiCl 4 is formed as by-product. This preactivated contact composition is mixed with unactivated silicon and used in the Müller-Rochow synthesis. This process makes it possible to produce concentrated contact compositions which are diluted with catalyst-free silicon before the alkylhalosilane synthesis. U.S. Pat. No. 6,528,674B1 describes a 2-stage process in which silicon is treated with a copper compound at a temperature below 500° C. In a second step, this pretreated contact composition is after-treated under inert gas at temperatures above 500° C. This contact composition which has been treated thusly is used in the Müller-Rochow synthesis for the production of dimethyldichlorosilane. WO 99/64429 describes a process for preparing alkylhalosilanes by reaction of a thermally pretreated contact composition with alkyl halide. The pretreatment comprises a reaction of silicon together with catalysts and promoters with carbon monoxide at temperatures in the range from 270 to 370° C., which results in an increase in the production rate.
[0011] DE102011006869 A1 describes a process in which silicon, copper compound, copper metal, zinc, zinc compound, tin, or tin compound, where at least the copper catalyst or promoter contains a chloride, are mixed to give a contact composition and the mixture is heated at a temperature in the range from 200° C. to 600° C. under a stream of carrier gas selected from among N 2 , noble gases, CO 2 , CO and H 2 , and used for the preparation methylchlorosilane.
[0012] The activation of the contact composition by means of a prereactor using HCl before the reaction with chloromethane is known, for example, from U.S. Pat. No. 4,864,044. There, a process in which silicon, copper catalyst, and optionally tin promoters but no zinc promoters, can be activated by means of HCl at about 325° C. is described in the examples. The disadvantages of this form of activation are that zinc or zinc compounds can be added only after the activation, since zinc reacts with HCl under the reaction conditions indicated to form readily sublimable zinc chloride and can thus be removed from the contact composition during the activation, and a dedicated reactor is necessary for the activation and the reaction products of the activation. In particular, trichlorosilane and tetrachlorosilane represent undesirable by-products of the methylchlorosilane synthesis. At least 1 to 2% of the silicon raw material used is consumed by the activation, and a relatively high activation temperature is required.
[0013] DE 19817775A1, too, states that fresh contact composition is not active enough. It should, for example, be activated by means of HCl.
[0014] There are further disadvantages of a separate pretreatment of the fresh contact composition. Fresh contact composition has to be heated to 370° C. for a certain time. This leads to high operational costs and capital costs. Steam is normally the heat source in industrial operations. A temperature of 300° C. can only be achieved using steam under extreme pressure, which is available in very few operations. Silanes, in particular chlorosilanes, are formed from CuCl and silicon during the preactivation and these have to be discharged and treated.
[0015] U.S. Pat. No. 2,389,931 describes reactor cascades (fluidized-bed reactors) in which greatly reacted contact composition from a reactor is separated off, cooled and introduced into a second reactor. This makes the silicon utilization more effective but very much more methyltrichlorosilane is formed as a result of the drastic reaction conditions. The contact composition also loses reactivity and selectivity due to the cooling.
SUMMARY OF THE INVENTION
[0016] The present invention provides a process for preparing methylchlorosilanes by reaction of chloromethane with a contact composition, wherein a mixture containing silicon, copper catalyst and promoter (contact composition 1) is fed into a first fluidized-bed reactor (fluidized-bed reactor 1), active contact composition (contact composition 2) is formed in the presence of chloromethane at from 200 to 450° C., part of the contact composition 2 is taken off from the fluidized-bed reactor 1, preferably via cyclones of the fluidized-bed reactor 1 preferably by means of reaction gas, preferably chloromethane, and fed into a second fluidized-bed reactor (fluidized-bed reactor 2) and reacted with chloromethane at from 200 to 450° C., where at least 20 parts by weight of contact composition 2 per 100 parts by weight of contact composition 1 are recirculated per unit time into fluidized-bed reactor 1 and the contact composition 2 which has been fed into the fluidized-bed reactor 2 and recirculated into fluidized-bed reactor 1 is not cooled below a temperature of 150° C. after being taken off from the fluidized-bed reactor 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] The contact composition 2 is significantly more active than a fresh contact composition (contact composition 1) and than a preactivated contact composition which has been activated under N 2 at, for example, about 300° C. The reaction of chloromethane with activated Si particles liberates energy. This leads to local temperature increases of up to several 100° C., and the surface is also freed of oxide layers and further passivating layers.
[0018] No separate apparatus has to be provided for the production of contact composition 2. It is possible to use the existing fluidized-bed reactors.
[0019] The fluidized-bed reactors 1 and 2 can be operated using different parameters such as pressure and temperature and thereby be adapted to the differences between the contact compositions 1 and 2 with different properties. Completely reacted contact composition is preferably discharged via a cyclone arranged downstream of the fluidized-bed reactor 2.
[0020] In a particular embodiment, the contact composition constituents (contact composition 3) discharged from the fluidized-bed reactor 2 or from the fluidized-bed reactors 1 and 2 with the gas stream is completely or partly recirculated into the fluidized-bed reactor 2. The contact composition 3 is preferably separated off from the gas stream using one or more cyclones.
[0021] The fluidized-bed reactor 1 is preferably operated at a higher temperature than the fluidized-bed reactor 2. Preference is given to the fluidized-bed reactor 1 being operated at 300-350° C. and fluidized-bed reactor 2 being operated at 250-300° C., with the temperature in the fluidized-bed reactor 1 preferably being higher. As a result, the fluidized-bed reactor 1 becomes more active and the fluidized-bed reactor 2 becomes more selective. This leads to overall better performances of the fluidized-bed reactors with greater selectivity with respect to dimethyldichlorosilane.
[0022] In a particular embodiment, further catalysts and/or promoters are added to the contact composition 2 taken off from the fluidized-bed reactor 1.
[0023] From 1 to 80% by weight, more preferably from 10 to 50% by weight, of the contact composition 1 fed into the fluidized-bed reactor 1 are preferably taken off per unit time from the fluidized-bed reactor 1 as contact composition 2 and fed into the fluidized-bed reactor 2.
[0024] In a particular embodiment, a plurality of, in particular, from 2 to 5, fluidized-bed reactors 1 are used. From 1 to 50% by weight, more preferably from 5 to 20% by weight, of the contact composition 1 fed in is preferably taken off as contact composition 2 from each of these fluidized-bed reactors 1 and fed into the fluidized-bed reactor 2.
[0025] From 30 to 50 parts by weight of contact composition 2 per 100 parts by weight of contact composition 1 are preferably recirculated per unit time into fluidized-bed reactor 1.
[0026] In a particular embodiment, the contact composition 2 taken off from one or more fluidized-bed reactors 1 is collected in a collection vessel and fed from the collection vessel into one or more fluidized-bed reactors 2.
[0027] In a particular embodiment, a plurality of, in particular from 2 to 5, fluidized-bed reactors 2 are used.
[0028] In a particular embodiment, the contact composition 2 is mixed with a thermally conductive material before it is fed into the fluidized-bed reactor 2. This improves the heat transfer of the contact composition particles (hot spots) at a heat removal system, for example a cooling finger.
[0029] The thermally conductive material is preferably selected from among silicon, silicon carbide or silicon dioxide, having a preferred particle size of 100-800 microns, more preferably 200-400 microns. Preference is given to mixing 100 parts by weight of contact composition 2 with up to 40 parts by weight, in particular with up to 20 parts by weight, of thermally conductive material.
[0030] The contact composition 2 fed into the fluidized-bed reactor 2 is preferably not cooled below a temperature of 180° C., in particular not below 200° C., after being taken off from the fluidized-bed reactor 1.
[0031] The contact composition 2 is preferably taken off from the fluidized-bed reactor 1 by means of reaction gas, preferably chloromethane. The contact composition 2 and optionally also the contact composition 3 is preferably fed into the fluidized-bed reactor 2 in a form which has been fluidized by means of chloromethane.
[0032] The silicon used in the process preferably contains not more than 5% by weight, more preferably not more than 2% by weight, and in particular not more than 1% by weight, of other elements as impurities. The impurities, which make up at least 0.01% by weight, are preferably elements selected from among Fe, Ni, Mn, Al, Ca, Cu, Zn, Sn, C, V, Ti, Cr, B, P, and O.
[0033] The particle size of the silicon is preferably at least 0.5 microns, more preferably at least 5 microns, and in particular at least 10 microns, and preferably not more than 650 microns, more preferably not more than 580 microns, and in particular not more than 500 microns.
[0034] The average particle size distribution of the silicon is the d50 value and is preferably at least 180 microns, more preferably at least 200 microns, and in particular at least 230 microns, and preferably not more than 350 microns, more preferably not more than 300 microns, and in particular not more than 270 microns.
[0035] The copper for the catalyst can be selected from among metallic copper, a copper alloy and a copper compound. The copper compound is preferably selected from among copper oxide and copper chloride, in particular CuO, Cu 2 O, and CuCl, and a copper-phosphorus compound (CuP alloy). Copper oxide can be, for example, copper in the form of copper oxide mixtures and in the form of copper(II) oxide. Copper chloride can be used in the form of CuCl or in the form of CuCl 2 , with corresponding mixtures also being possible. In a preferred embodiment, the copper is used as CuCl.
[0036] Preference is given to using at least 0.1 parts by weight, more preferably at least 1 part by weight, of copper catalyst and preferably not more than 10 parts by weight, in particular not more than 8 parts by weight, of copper catalyst, in each case based on metallic copper, per 100 parts by weight of silicon.
[0037] The contact composition 1 preferably contains a zinc promoter which is preferably selected from among zinc and zinc chloride. Preference is given to using at least 0.01 parts by weight of zinc promoter, more preferably at least 0.1 parts by weight of zinc promoter, and preferably not more than 1 part by weight, in particular not more than 0.5 parts by weight, of zinc promoter, in each case based on metallic zinc, per 100 parts by weight of silicon.
[0038] The contact composition 1 preferably contains a tin promoter which is preferably selected from among tin and tin chloride. Preference is given to using at least 0.001 parts by weight of tin promoter, more preferably at least 0.05 parts by weight of tin promoter, and preferably not more than 0.2 parts by weight, in particular not more than 0.1 parts by weight, of tin promoter, in each case based on metallic tin, per 100 parts by weight of silicon.
[0039] The contact composition 1 preferably contains a combination of zinc promoter and tin promoter, and in particular additionally contains a phosphorus promoter.
[0040] Preference is given to at least 30% by weight, in particular at least 50% by weight, of the total of copper catalyst and promoters being chlorides of copper, zinc and tin.
[0041] Apart from the zinc and/or tin promoters, it is also possible to use further promoters which are preferably selected from among the elements phosphorus, cesium, barium, manganese, iron and antimony and compounds thereof.
[0042] The P promoter is preferably selected from among CuP alloys.
[0043] The pressure in the reaction is preferably at least 1 bar, in particular at least 1.5 bar, and preferably not more than 5 bar, in particular not more than 3 bar, in each case reported as absolute pressure.
[0044] The methylchlorosilanes prepared are, in particular, dimethyldichlorosilane, methyltrichlorosilane, trimethylchlorosilane and H-silanes.
[0045] The process can be carried out batchwise or preferably continuously. Continuously means that silicon which has reacted and possibly catalysts and promoters discharged with the reaction dust are continually replaced, preferably as premixed contact composition 1 and contact composition 2 and optionally contact composition 3. Preference is given to chloromethane being simultaneously introduced as a reactant and fluidizing medium into the fluidized-bed reactors 1 and 2.
[0046] In the following examples, all amounts and percentages are, unless indicated otherwise in the particular case, by weight, all pressures are 0.10 MPa (abs.) and all temperatures are 20° C.
EXAMPLES
[0047] I) Examination of the Performance of Contact Composition 2:
1. 50 g of contact composition 2 from an industrial fluidized-bed reactor are reacted with about 20 l/h of chloromethane at 340° C. in a laboratory fluidized-bed reactor. After a reaction time of 7 hours, 103 g of crude silane had been obtained with a dimethyldichlorosilane selectivity of 71% (73 g of dimethyldichlorosilane). 2. 280 ppm of P were added to 50 g of contact composition 2 from an industrial fluidized-bed reactor and reacted with about 20 l/h of chloromethane at 340° C. in a laboratory fluidized-bed reactor. After a reaction time of 7 hours, 93 g of crude silane had been obtained with a dimethyldichlorosilane selectivity of 78% (73 g of dimethyldichlorosilane). The addition of P to contact composition 2 leads to a lower activity but an increase in the selectivity, so that ultimately the same amount of dimethyldichlorosilane is produced with a significantly smaller amount of secondary silanes. 3. 50 g of contact composition 2 from an industrial fluidized-bed reactor were reacted with about 20 l/h of chloromethane at 320° C. in a laboratory fluidized-bed reactor. After a reaction time of 7 hours, 86 g of crude silane had been obtained with a dimethyldichlorosilane selectivity of 74% (64 g of dimethyldichlorosilane). The temperature decrease does lead to a lower activity but to better selectivity.
II) Examination of the Performance of 50% of Contact Composition 2+50% of Contact Composition 1:
[0000]
25 g of contact composition 2 from an industrial fluidized-bed reactor together with 25 g of contact composition 1 were reacted with about 20 l/h of chloromethane at 340° C. in a laboratory fluidized-bed reactor. After a reaction time of 7 hours, 33 g of crude silane had been obtained with a dimethyldichlorosilane selectivity of 76% (25 g of dimethyldichlorosilane).
The addition of contact composition 1 leads to a significantly lower activity. | Methylchlorosilanes are synthesized by an at least two stage reaction in which contact composition from a first fluidized bed reactor is fed to a second fluidized bed reactor. | 1 |
BACKGROUND OF THE INVENTION
The invention disclosed and claimed herein generally pertains to a method of magnetic resonance (MR) imaging, wherein acquired MR data has an associated linear phase shift which must be determined to reduce image artifacts, improve image quality or as a measure of some physical quantity. More particularly, the invention pertains to a method of the above type which significantly improves or enhances efficiency in determining linear phase shift. Even more particularly, the invention pertains to a method of the above type wherein MR data is acquired in one domain, such as the time domain, and the associated linear phase shift is determined in a domain conjugate thereto, such as the frequency domain.
As is well known by those of skill in the art, acquired MR image data may comprise complex valued signals, such as data acquired by sampling an MR signal in quadrature. Each data sample then comprises a complex value having an associated magnitude and phase. Complex valued signals are often considered to have two equivalent representations, referred to as the time domain and frequency domain representations, respectively.
As is further well known, certain MR imaging techniques require determination of linear or first order phase shift, that is, the variation of phase between adjacent MR data samples in a set of MR data. For example, linear phase shift is used in connection with a technique known as navigator echo, to determine the position of selected body structure of a patient which is subject to periodic or cyclical respiratory motion. Such positional information is essential, in order to minimize artifacts in providing an image of the moving structure. Typically, body structure associated with respiration comprises a patient's diaphragm, as well as organs such as the lungs and liver which move with the diaphragm. Such information is particularly useful for coronary artery MR imaging and general abdominal body MR imaging.
One such navigator echo technique, described in an article by Foo et al entitled “Navigator and Linear Phase Shift Processing”, Proceedings of ISMRM, page 323 (1998), is based on the Fourier Transform Shift Theorem. Such technique is also described in U.S. patent application Ser. No. 08/980,192, filed Nov. 26, 1997 by Foo et al, and issued as U.S. Pat. No. 6,067,465 on May 23, 2000, which is commonly assigned herewith to the General Electric Company. In accordance with the Fourier Transform Shift Theorem, if an object centered about the origin of a coordinate system is displaced in a specified direction, then the Fourier transform of a function defining the object will have a linear phase shift that is equivalent to the amount of spatial displacement. Thus, in the Foo et al technique, a navigator echo signal associated with a moving structure of interest is acquired in the time domain. The acquired navigator echo is then Fourier transformed into the frequency domain, to provide a corresponding frequency profile or spectrum. The spectrum is truncated or apodized, such as by means of a band limiting filter, to remove any extraneous signal components. The truncated frequency profile is then Fourier transformed back to the time domain. Thereupon, linear phase shift is determined in the time domain, preferably by means of the Ahn algorithm. The position of the structure of interest, at the acquisition time of the navigator echo, may then be readily computed. The Ahn algorithm is a very well known technique for determining linear phase shift of a complex valued signal, and is described, for example, in “A New Phase Correction Method in NMR imaging based on Auto Correlation and Histogram Analysis”, Ahn, et. al., IEEET Trans. Med. Imaging, 1987: MI-6: 32-36.
While the Ahn algorithm is known to be very computationally efficient, it will be seen that the navigator echo technique described above requires a Fourier transformation operation, from the frequency domain back to the time domain, before the Ahn algorithm can be applied. It would significantly enhance computational efficiency even further, if linear phase shift could be determined directly from frequency domain data so that the transformation back to the time domain would be unnecessary. In addition, certain multi-echo image sequences, such as echo planar imaging (EPI) and fast spin echo (FSE), also require determination of linear phase shift of the frequency domain spectrum (obtained from the time domain echo signal by Fourier transformation), for use in phase correction. In certain applications associated with these sequences, linear phase shift must be computed in near-real time, in order to provide phase correction of the multi-echo signals as image acquisition and reconstruction is being carried out. For these applications also, it would be very useful to be able to determine linear phase shift from data directly available in one domain, and to thus avoid the need to perform a Fourier transform back to the other domain. Significant reduction in processing time could thereby be achieved.
SUMMARY OF THE INVENTION
The invention provides a method for estimating or determining the linear phase shift of an MR signal with a level of computational efficiency which is comparable to the Ahn algorithm. It is particularly suitable to implementation in real-time signal processing applications. The method can be applied to the Discrete Fourier Transform ( DFT) of the samples that are employed in Ahn calculations. It is therefore assumed that the method will be of particular use when the sampled data exists in a domain which is conjugate to the domain for which the linear phase shift of the data is to be determined, and where an additional DFT would otherwise be required to evaluate the Ahn formula. It is considered to be entirely complementary to the existing Ahn procedure, while eliminating need for the additional DFT.
The method of the invention includes the step of applying an MR sequence to an object of interest, to acquire a set of complex valued MR data samples having an associated linear phase shift in a specified domain. The method further comprises generating a set of conjugate data samples, in a domain which is conjugate to the specified domain, from the acquired data samples. The linear phase shift is determined from the conjugate data samples, by means of computations which are executed or carried out exclusively in the conjugate domain, the linear phase shift then being employed to reduce artifacts in constructing an MR image of the object. In one useful embodiment, the set of acquired data samples is acquired in the time domain, and the generating step comprises applying a Fourier transform to the acquired data samples, to provide conjugate data samples which are in the frequency domain. However, the invention is not limited thereto.
In a preferred embodiment of the invention, the determining step comprises the steps of convolving adjacent conjugate data samples to provide a specified function, and then computing the value of the function at a specified spectral frequency to determine linear phase shift. Preferably, the spectral frequency is selected to be zero. Embodiments of the invention may be usefully employed to reduce artifacts in connection with navigator echo techniques, and also in multi-echo imaging sequences.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic diagram showing basic components of an MR system for use in practicing an embodiment of the invention.
FIG. 2 is a flowchart showing the Ahn procedure in the time domain.
FIG. 3 is a flowchart showing a procedure, comprising an embodiment of the invention, in the frequency domain.
FIG. 4 is a graph showing a magnitude-squared signal in the frequency domain which is associated with the embodiment of FIG. 3 .
FIG. 5 is a diagram representing the data depicted in FIG. 4 in the complex plane.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, there are shown the basic components of an MR system or scanner 10 which may be operated to acquire MR data in accordance with the invention described herein. System 10 includes an RF transmit coil 12 , as well as a cylindrical magnet 14 for generating a main or static magnetic field B 0 in the bore thereof. RF coil 12 is operated to transmit RF excitation signals into a patient or other subject of imaging 16 residing in the magnet bore, in order to produce MR signals. System 10 further includes gradient coils 18 , 20 and 22 for generating G x , G y , and G z magnetic field gradients relative to orthogonal X-, Y- and Z-reference axes, respectively. FIG. 1 shows each of the gradient coils 18 , 20 and 22 respectively driven by gradient amplifiers 24 , 26 and 28 , and RF coil 12 driven by transmit amplifier 30 . FIG. 1 further shows an RF coil 32 , which is operated in association with a receive amplifier 34 to acquire MR signals from subject 16 . In some arrangements, coil 32 and coil 12 comprise the same RF coil, which is operated in alternate modes during the imaging sequence. System 10 is further provided with a pulse sequence control 36 , which is operated to control the RF and gradient amplifiers, and to thereby generate pulse sequences to produce and acquire sets of MR signals. System 10 also includes system control and data processing electronics 38 for operating respective components of system 10 to acquire MR data, to process the data in accordance with the invention, and to construct images therefrom. The construction, functions, and interrelationships of components of MR system 10 are well known and described in the prior art, such as in U.S. Pat. No. 5,672,969, issued Sep. 30, 1997 to Zhou et al.
Referring further to FIG. 1, there is shown patient 16 supported on a table 40 or the like so that the chest and cardiac region 42 of the patient is positioned within the bore of main magnet 14 . The patient's diaphragm, as well as anatomic structure attached thereto such as the liver and lungs, moves along an axis R, during the course of successive respiratory cycles. Thus, displacement of the diaphragm and related structure, with respect to a reference position, varies periodically as a function of time. For purposes of description, the axis R is usefully considered to lie along the Z-axis of scanner 10 .
As stated above, the navigator echo technique is very useful in MR imaging, such as in 3D MR coronary artery imaging or general abdominal body MR imaging, to determine the position of a patient's diaphragm. If the diaphragm is within a specified positional window (i.e., a particular range of positions relative to a reference position) when an MR image sequence is applied thereto, MR data produced by the sequence will be accepted for use in image reconstruction. Otherwise, the data will not be accepted. As also stated above, linear phase shift of a navigator echo, which is generated by a navigator pulse included in the image sequence, is computed by means of the Ahn algorithm, in order to provide a measurement of diaphragm displacement.
The Ahn algorithm provides a simple algorithm to calculate an estimate of the first order phase of a complex valued signal f(t), given samples f T , where T=0, . . . , N−1. The algorithm provides an estimate of the first order phase in the form of the linear phase shift per sample (i.e. the phase shift, δφ between f T and f T+1 ) as follows: δ φ = arg [ ∑ T f T + 1 f T * ] Eqn . ( 1 )
Equation (1) can be understood by recognizing that each (complex valued) sample may be written as f T =A T exp(iφ T ). For each T, an estimate of the phase shift per sample δφ is provided by δφ=φ T+1 −φ T . The product f T+1 f* T is set forth as follows:
f T+1 f* T =A T A T+1 exp[ i (φ T+1 −φ T )]= A T A T+1 e iδφ T Eqn. (2)
In Eqn. (2), (*) denotes complex conjugation, and the product is a complex number with phase δφ T and magnitude that is approximately the square of the local signal amplitude. (In fact, it is the square of the geometric mean of the two signal samples.) The Ahn method provides an estimate of δφ from the phase of the complex sum of these product terms.
The implicit magnitude squared weighting enhances the robustness of the Ahn method, since samples with low relative amplitude and, assuming uniformly distributed noise, low SNR are effectively suppressed. The method also avoids problems with phase wrapping, when the signal phase extends over a range in excess of 2π. The method is also extremely efficient computationally: given complex samples as pairs of real and imaginary values, the algorithm requires only 4N (real) multiplications, 4N (real) additions and a single arctan computation.
In the previously described navigator echo technique, the Ahn algorithm operates on data in the time domain to determine linear phase shift δφ, in accordance with Equations (1) and (2). This operation is illustrated by the flowchart of FIG. 2 . As shown therein, g T , which is the product of f T+1 f* T , is summed over all sample times T. δφ is then derived as the argument of such summation.
Notwithstanding advantages of the Ahn algorithm, it has been recognized, in accordance with the invention, that it would be very desirable to provide an alternative method for detecting linear phase shift. More specifically, it could be highly beneficial to determine linear phase shift in a domain conjugate to the domain in which MR data is acquired, and at the same time to provide a level of computational efficiency which is comparable to the Ahn algorithm. As stated above, such method would reduce MR signal processing effort by eliminating need for certain Fourier transform operations.
In order to develop such method, further reference is made to Equation (1), wherein the term inside the summation (i.e., f T+1 f* T ) may be interpreted as a pointwise multiplication of a time-shifted signal f′ T =f T+1 , and the complex conjugate of the original signal. These products are then summed over all the samples (i.e. the full extent of the sampled signal). Such pointwise multiplication, of a shifted copy of the time domain signal f T+1 with the complex conjugate of the original time domain signal f* T gives g T =f T+1 f* T , as shown in FIG. 2 .
The time-shifted signal in the time domain corresponds to a linear phase shifted spectrum in the frequency domain, while the complex conjugate signal corresponds to the complex conjugate of the frequency reversed spectrum. Accordingly, the pointwise multiplication in the time domain corresponds to a convolution in the frequency domain as follows:
g T =f T+1 f* T →( F k e i2πk/N ) {circle around (x)} ( F* −k ) Eqn. (3)
(
F
k
2
π
k
/
N
)
⊗
(
F
-
k
*
)
=
1
N
∑
k
′
=
0
N
-
1
F
k
′
2
π
k
′
/
N
F
-
(
k
-
k
′
)
*
=
G
k
Eqn
.
(
4
)
In Eqn. (3), the arrow represents the Fourier transform operation, from the time domain into the frequency domain. In Eqns. (3) and (4), k represents the k th sample or spectral frequency, k=0, . . . , N−1, F k is the magnitude thereof, and 2πk/N is the phase thereof.
In accordance with the invention, it has been recognized that summation over all samples in the time domain, that is, summation of all values as referred to above, corresponds to evaluation of the spectrum, in the frequency domain, at the specific frequency k=0. This provides the following relation: ∑ T = 0 N - 1 g T = N G O Eqn . ( 5 )
Eqns. (4) and (5) provide the following relation: N G O = ∑ k ′ = 0 N - 1 ( F k ′ F k ′ * ) 2 π k ′ / N = ∑ k = 0 N - 1 F k 2 2 π k / N Eqn . ( 6 )
From the flowchart of FIG. 2 it is seen that δφ can be determined from ∑ T = 0 N - 1 f T + 1 f T * ,
which is equal to ∑ T = 0 N - 1 g T .
From Eqn. (5), it is seen that ∑ T = 0 N - 1 g T ,
in the time domain, is equivalent to {square root over (N)}G O , in the frequency domain. Given such equivalency, together with Eqn. (6), linear phase shift δφ, the phase shift per sample, can be determined in the frequency domain from the following relationship: δ φ = arg [ ∑ k = 0 N - 1 F k 2 2 π k / N ] Eqn . ( 7 )
From Eqn. (7), linear phase shift can be determined exclusively from MR data samples in the frequency domain. Referring to FIG. 3, there is shown a flowchart which sets forth respective steps in deriving Eqn. (7). It will be seen that calculation of δφ therefrom involves the calculation of the squared magnitude at each sample point k, multiplication by a complex phasing factor and summation of the resulting complex values.
Since the phasing coefficients (e i2πk/N ) for Eqn. (7) can be precalculated (for any given N), linear phase shift δφ can be computed with a high level of efficiency. The coefficients can be stored as a table of cosine and sin values for each value of k, and the squared magnitude at each sample point is calculated as the sum of the squares of the real and imaginary components of F k . This value is then multiplied by the appropriate cosine and sin coefficients and accumulated. Thus, the conjugate algorithm, as set forth in Eqn. (7), has similar efficiency to the original Ahn formulation, requiring only 4N (real) multiplications, 3N (real) additions and a single arctan computation. However, it is unnecessary to Fourier transform respective data samples back to the time domain, as is required for a number of important applications of the Ahn algorithm.
In Equation (7), (F k ) k=0 N−1 is the spectrum of the signal (f T ), and the term |F k | 2 is simply the magnitude squared at a given point k. Referring to FIG. 4, there is shown a graph comprising a plot of |F k | 2 versus k, having peaks 44 , 46 , and 48 . Each value |F k | 2 is given a phase angle 2πk/N by multiplication with the complex exponential term. Such data can alternatively be represented as a fan of vectors in the complex plane, at equally spaced angles as k varies. The process can be interpreted as wrapping a magnitude squared profile around the unit circle in the complex plane. This is depicted in FIG. 5, which shows vectors 52 in the complex plane 50 . Finally, the complex sum of superposition of the vectors is determined, and the argument of the resultant is evaluated.
The peaks labeled 44 , 46 and 48 in the graph of FIG. 4 respectively correspond to the similarly labeled bulges in FIG. 5 . The bold vector 54 indicates the direction of the resultant of the superposition of the vectors, and is determined to provide δφ.
In a modification of the invention, MR data could be provided in the frequency domain, and linear phase shift could be determined, in accordance with Equation (7), in the time domain.
Obviously, other modifications and variations of the present invention are possible in light of the above teachings. It is therefore to be understood that within the scope of the disclosed concept, the invention may be practiced otherwise than as specifically described. | A method is provided for estimating or determining the linear phase shift of an MR signal pertaining to an object of interest. In accordance with the method, an MR sequence is applied to the object, to acquire a set of MR data samples in a specified domain, such as the time domain, the acquired data samples having an associated linear phase shift. A set of conjugate data samples is generated from the acquired data samples, in a domain conjugate to the specified domain such as the frequency domain. The linear phase shift is then determined from the conjugate data samples, by means of computations which are executed exclusively in the conjugate domain. The efficiency of such computations is comparable to the efficiency of the Ahn algorithm. The resultant linear phase shift is employed to reduce artifacts in constructing an MR image of the object, in connection with an MR technique such as navigator echo, or multi-echo imaging. | 0 |
TECHNICAL FIELD
[0001] This invention relates to electrolysis. More specifically, this invention relates to an improved method and apparatus for dissociating water to produce hydrogen and oxygen.
BACKGROUND OF THE INVENTION
[0002] The first electric battery was described in a letter from Volta dated Mar. 20, 1800 to the President of the Royal Society, Sir Joseph Banks ‘On the electricity excited by the mere contact of conducting substances of different kinds’. Shortly thereafter, Anthony Carlisle and William Nicholson replicated Volta's experiments. Because they sought to use a doubler to show charges on the upper and lower plates, they had to connect them to the electroscope, and it was not easy to maintain a good contact. To overcome this problem they added a drop of water to the uppermost disc and inserted the wire into the drop. They were surprised to note the appearance of a gas, soon shown to be hydrogen. They then took a small tube filled with water from the New River (an artificial channel completed in 1613 to bring water from Hertfordshire to the City) and inserted wires from the Voltaic pile at each end. To their astonishment the other suspected constituent of water, oxygen, did not appear at the same place but at the other wire ‘at a distance of almost two inches’. They had discovered electrolysis. The present invention is an improvement on that process.
[0003] In 2005, the United States Department of Energy (DOE) updated its goals for hydrogen production. The DOE noted that one kilogram of hydrogen contains approximately the same energy as one gallon of gasoline, termed as a “gallon of gasoline equivalent,” or “gge.” The DOE therefore set the goal for the DOE's hydrogen program to develop methods and techniques capable of producing hydrogen for between $2-$3 in 2005 dollars per gge by 2015. In the intervening three years, the DOE has funded millions of dollars of research at universities and DOE owned federal laboratories to attain this goal. To date, no one has reported any results that have done so. Accordingly, there is a long felt need by those having ordinary skill in the art to devise less expensive methods and apparatus for making hydrogen that will meet the DOE goal. The present invention provides such a method and apparatus.
SUMMARY OF THE INVENTION
[0004] The present invention is a method and apparatus for dissociating water into its elements. The present invention is shown in FIG. 1 . As shown, the invention provides a reaction chamber 1 , an anode 2 , a cathode 3 , and an aqueous hydroxide electrolyte 4 positioned between the anode and the cathode in the reaction chamber. The temperature of the aqueous hydroxide electrolyte in the reaction chamber is elevated to least 280° C. The pressure of the aqueous hydroxide electrolyte in the reaction chamber is likewise elevated to least 2 atmospheres. As used herein, an “aqueous hydroxide electrolyte” is a solution of water and a hydroxide electrolyte. An electrical voltage is applied across the anode 2 and cathode 3 using an electrical power supply 5 . The resulting electrolysis of the water in the aqueous hydroxide electrolyte produces hydrogen and oxygen gas, and does so more efficiently that any electrolytic process described in the prior art. As hydrogen and oxygen are evolved from the anode and cathode, additional water, preferably in the form of steam, may be added to the aqueous hydroxide electrolyte 4 to provide a fresh source of hydrogen and oxygen for the reaction. The process of adding additional water may be performed as a continuous or as a batch process.
[0005] Preferably, to protect against corrosion, the reaction chamber 1 is formed of, or coated with, a protective metal. Suitable metals include nickel, titanium, zirconium, molybdenum, chromium, platinum, gold, palladium, copper, cobalt, silicon, alloys containing the forgoing, and combinations thereof. Preferably, the hydroxide electrolyte 4 consists of alkaline hydroxides and alkaline earth hydroxides, and combinations thereof. Suitable alkaline hydroxides are LiOH, KOH, NaOH, CsOH, RbOH, and combinations thereof. Suitable alkaline earth hydroxides are Ba(OH) 2 , Sr(OH) 2 , Mg(OH) 2 , Ca(OH) 2 , and combinations thereof. Preferably, to protect against corrosion, the anode 2 and the cathode 3 are formed or coated with a noble metal. Suitable noble metals include palladium, platinum, and gold.
[0006] A preferred embodiment of the present invention is shown in FIG. 2 . As shown, multiple anodes 2 and cathodes 3 are submerged in the aqueous hydroxide electrolyte 4 . A plurality of separator plates 6 are interposed between the multiple anodes and cathodes to keep hydrogen and oxygen formed at the anodes 2 and cathodes 3 separated from one and another. Preferably, the separator plates are made a corrosion resistant material, or with a corrosion resistant coating. The lower portion of the separator plates 6 are submerged in the aqueous hydroxide electrolyte 4 and are configured as a solid barrier with perforations. In this manner, the separator plates provide fluid pathways to allow transfer of hydroxide ions from adjacent anodes 2 and cathodes 3 , prevent bubbling oxygen and hydrogen evolving from adjacent anodes 2 and cathodes 3 from mixing. The upper portion of the separator plates 6 are not submerged in the aqueous hydroxide electrolyte 4 and are configured as a solid barrier with no perforations, to prevent oxygen and hydrogen evolving from adjacent anodes 2 and cathodes 3 from mixing in the space above the aqueous hydroxide electrolyte 4 .
[0007] Another preferred embodiment of the present invention is shown in FIG. 3 . A pump 11 is used to pressurize water 19 to a pressure greater than 2 atm 20 . A mixing pipe 12 combines recycled water streams with feed water and is preheated in heat exchangers 13 and 14 . Additional heat required to bring the water to the appropriate electrolysis temperature is added by another heat source 15 to produce superheated steam 21 . This superheated steam is provided to the reaction chamber 1 of the present invention which produces mixed streams of oxygen and water 22 and hydrogen and water 25 . Each stream is cooled by the water preheaters 13 and 14 and is fed to separation tanks 17 and 18 to produce streams of pressurized water 23 and 26 along with pressurized oxygen 24 and pressurized hydrogen 27 .
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The following detailed description of the embodiments of the invention will be more readily understood when taken in conjunction with the following drawings, wherein:
[0009] FIG. 1 is a schematic drawing of the present invention as previously described in the summary of the invention.
[0010] FIG. 2 is a schematic drawing of one aspect of a preferred embodiment the present invention as previously described in the summary of the invention.
[0011] FIG. 3 is a schematic drawing of an additional aspect of a preferred embodiment the present invention as previously described in the summary of the invention.
[0012] FIG. 4 is a schematic drawing of an alkaline electrolysis cell used in the proof of principle experiments described herein.
[0013] FIG. 5 is a graph showing the polarization behavior of the alkaline electrolysis cell used in the proof of principle experiments described herein operating under an open atmosphere at 200° C., 250° C., 300° C., 350° C., 400° C., and 450° C.
[0014] FIG. 6 is a graph showing the power production performance of the an alkaline electrolysis cell used in the proof of principle experiments under a self-generated steam pressure described herein operating at 200° C., 250° C., 300° C., 350° C., 400° C., and 450° C.
[0015] FIG. 7 is a graph showing a comparison of measured alkaline electrolysis cell pressures and the pressure of saturated steam at various temperatures. The trend line for saturated steam is extrapolated beyond the data available in commercial steam tables.
[0016] FIG. 8 is a graph showing a comparison of various anode compositions tested in the alkaline electrolysis cell at 400° C. and elevated pressure.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] For the purposes of promoting an understanding of the principles of the invention, a series of experiments were conducted reducing the present invention to practice. These experiments demonstrated the direct-current electrolysis of potassium hydroxide solutions at temperatures (up to 400° C.) and under various pressures. One example of a high-temperature alkaline electrolysis cell resistant to chemical attack from the highly corrosive electrolyte solution and capable of high pressure operation was designed and tested. The cell was constructed with a Monel® (66.5% Ni, 31.5% Cu, 1.2% Fe, 1.1% Mn) alloy housing and cathode, while various anode materials were compared. The anode materials tested included nickel, Monel® alloy, lithiated nickel, and cobalt-plated nickel. Preferred anode materials are conductive metals resistant to corrosive attacks by alkaline electrolytes. More preferred are these materials configured as having a high surface area to volume ratio, as is found in nano-engineered and catalytic materials. The advantages of operating an alkaline electrolysis cell at high temperatures include increasing the ionic conductivity of the electrolyte and enhancing the rates of surface chemical reactions at the electrode surfaces. Cell operation with high steam partial pressures above the solution is also shown to enhance cell performance. The prudent selection of anode material also impacts the cell polarization and consequently the cell power efficiency. The best cell performance was achieved using a cobalt-plated nickel anode at a temperature of 400° C. and a steam partial pressure of 8.7 MPa.
[0018] A cutaway schematic for the high-temperature, high-pressure alkaline electrolysis cell is shown in FIG. 4 . The cell container was machined from 7 cm diameter Nickel bar stock cut to 15 cm in length. Nickel-400, also known as the commercial Monel® alloy, was chosen due to its resistance to corrosion by high-temperature alkali hydroxide solutions. The bar was internally bored to a depth of 11 cm with a diameter of approximately 3.8 cm. This central well served to store the electrolyte solution. The cell was heated by three 200 W cartridge heaters inserted into the bottom of the container. The top of the cell container was machined with a knife edge and bolt holes designed to mate with a standard 7 cm stainless steel Conflat® flange with a copper gasket, which served as a cap for the container. The cap provided three conduits: electrically isolated anode and cathode ports and a combined thermocouple port and steam vent, on which a needle valve and a high pressure steam gauge were each installed. The steam pressure gauge was protected by attachment to a short siphon tube which was charged with a small amount of distilled water prior to use.
[0019] The electrolyte used at the beginning of each experimental set (initially at room temperature) was a 19 M potassium hydroxide (KOH) solution prepared by mixing appropriate amounts of KOH purchased from Alfa Aesar with distilled water. Direct current electrical power was provided to the electrolysis cell using a digital power supply (Aglient Technologies, model E3617A). The power supply was placed in current-control mode at several pre-determined total electrical current increments ranging from 50 mA to 1000 mA, and the corresponding terminal voltage was measured and recorded using a digital multimeter (Extech Instruments, model 470). The electrolysis cell was allowed to stabilize at each current density for at least five seconds before the terminal voltages were measured and recorded. The resulting data was incorporated into polarization, or i-V, curves for each experimental set.
[0020] This design proved to be reliable for high cell operating temperatures and the associated elevated steam pressures without leaking. The cell was operated over a range of temperatures from 35° C. to 400° C. and total pressures from atmospheric to nearly 9 MPa.
[0021] The anode and cathode used in each experiment were solid metal wires 3.2 mm in diameter. The cathode in each experiment was Monel® wire, while several anode compositions were investigated in an attempt to mitigate electrode polarization, enhance surface reaction rates, and minimize corrosion. Anodic electrodes in electrolytic devices exist under relatively oxidizing conditions with respect to other locations within the cell, and as such are more prone to corrosion and polarization. This effect is most often observed as an increased overall electrolytic potential, which in turn leads to a decreased energy efficiency of the cell. The anode types tested in the present study included nickel (Alfa Aesar), Monel® (McMaster-Carr), lithiated nickel, and cobalt-plated nickel.
[0022] To produce the lithiated nickel anodes—which were nickel wires coated lithium-doped nickel oxide using a thermal-electrochemical treatment procedure. Nickel wire was treated in a 3 M LiOH solution maintained at 100° C. for 24 hours while applying an anodic current of 1 mA cm −2 . In this single-step treatment, nickel metal is thermally and electrochemically converted first into a hydrated nickel oxide, which is further electrochemically oxidized and lithiated by cationic exchange to produce stoichiometric variants of LiNiO 2
[0023] The cobalt-plated nickel anodes were produced by electroplating cobalt on bare nickel wires at a current density of 10 mA cm −2 for 1 hour from a 0.05 M solution of cobalt (II) sulfate with a supporting electrolyte of sodium sulfate and sodium citrate at concentrations of 0.1 M and 0.25 M, respectively. All chemicals used in the cobalt plating solution were purchased from Alfa Aesar. After electroplating, the electrode was observed to have a dull gray color. Each cobalt-plated electrode was gently polished by hand with wet 1200 grit silicon carbide paper in order to remove dendrites and any other plating irregularities that might magnify the electrode surface area.
[0024] The electrode wires were isolated from one another and the cell housing by compression fitting-sealed Teflon® tubing sleeves, with a supplemental external wrapping of Teflon® tape at tubing and wire junctions, at the top of each electrode. The sleeves were placed approximately three centimeters above the cell cap. During cell operation, the upper region of each electrode was cooled externally by flowing tap water to prevent melting and failure of the Teflon® sleeves. While immersed in the electrolyte, each electrode was submerged to a depth of 5 cm, which corresponded to approximately 5 cm 2 of exposed electrode area for each wire. The two electrodes were separated by a lateral center-to-center distance of 1 cm.
[0025] The first series of experiments involved the measurement of electrolyzer performance while the electrolyte was exposed to ambient air. In each of these experiments, the ambient temperature was maintained at 22° C. and a relative humidity of 40% using laboratory climate controls. The atmospheric pressure naturally varied between 100 and 102 kPa. As cell temperature was adjusted from low to high, at least two hours were allowed for the electrolyte solution to establish equilibrium with the surrounding air. This was especially important at higher temperatures, where the potassium hydroxide solution would tend to quickly dehydrate with the rapid temperature step increase, and then slowly re-hydrate to a limited extent through contact with the surrounding humid air. Additionally, as the volume of the electrolyte would vary with temperature, the vertical position of each electrode was adjusted as necessary to maintain a 5 cm immersion depth. A polarization curve was created for the system at several temperatures. In each experiment at atmospheric pressure, both the anode and cathode were Monel® wires.
[0026] A series of electrolysis experiments involving elevated pressure over the KOH solution were carried out in the following way. At room temperature, the electrolysis cell was filled to the desired level with 19 M KOH solution and was tightly sealed. The unwetted space above the electrolyte, including the volume of the steam siphon tube, comprised a volume of approximately 50 cm 3 . A polarization curve was created for the system as described above. When each polarization curve was completed, the anode and cathode were electrically shorted in order to return the cell to electrical equilibrium as the cell temperature was raised to the next prescribed level. Electrical currents of several amperes were observed for short periods of time as the small amount of hydrogen and oxygen gases within the cell reacted, as in a fuel cell, to form water once again. When the cell reached the next temperature to be tested and the short circuit current had returned to zero, the total gas pressure over the melt was recorded. The partial pressure of steam above the electrolyte was estimated as the specific gauge pressure displayed. The polarization measurements were then repeated at the current temperature. The entire measurement process was repeated until all process temperatures had been investigated. The set of experiments at elevated pressure covered a range of temperatures from 35° C. to 400° C. and utilized Monel® electrodes only.
[0027] The attempt to reduce electrode polarization, enhance surface reaction rates, and minimize corrosion by changing the electrode material was one of optimization, and therefore a single operating condition for the electrolysis cell was chosen to compare the effects of the different electrodes on cell performance. Specifically, the four types of anodes (nickel, Monel®, lithiated nickel, and cobalt-plated nickel) were examined with the cell sealed and operating at 400° C. Data was collected in the same manner detailed above for obtaining polarization curves at elevated pressure.
[0028] Polarization curves of the electrolysis cell operating between 200° C. and 400° C. under an open atmosphere are shown in FIG. 5 . The general trend of reduced electrolytic voltage with increasing temperature is apparent, although it appears that the compounded magnitude of this effect is reduced at higher temperatures. Electrolyte ionic conductivity and surface reaction rates are expected to increase with temperature, and additionally the reversible cell potential for water splitting is known to thermodynamically decrease as temperature rises. The limit of cell performance improvement with increasing temperature is likely due to a combination of electrode oxidation/deactivation and a lower water activity in the solution as it becomes dehydrated. Accordingly, it is preferred that water be continually provided to the electrolyte. The concept of maintaining a high pressure of steam over the solution was introduced to the present study as a means to force water into the solution at high temperature, and to ensure its high activity within the solution.
[0029] Polarization curves of the sealed electrolysis cell operating between 35° C. and 400° C. under a self-generated equilibrium steam pressure are shown in FIG. 6 . The improvement in apparent electrolysis effectiveness with respect to open-atmosphere tests is striking. Although the reversible cell potential for the electrolysis of water is above 900 mV for all temperatures up to about 415° C., an applied voltage of less than 500 mV was required to provide 200 mA cm −1 at 400° C. under high steam pressure. A reduced voltage was expected due to the high water activity within the electrolyte, its impact on system free energy and equilibrium, and the consequent substitution of electrical energy with thermal energy.
[0030] An interesting illustration of the alkaline solution's affinity for water is displayed in FIG. 7 . Here, the measured gauge pressure over the electrolyte at various temperatures is shown in comparison to the saturation pressure of steam at the same temperature. The cell pressure was measured at several points intermediate of polarization measurements in order to obtain a clear trend. Cell temperatures of up to 400° C. would not have been possible without the high temperature hygroscopic nature of the alkaline solution.
[0031] Cobalt-plated nickel wires were examined for their ability to reduce electrode polarization, enhance surface reaction rates, and minimize corrosion. Nickel and Monel® wires were used as received, while the lithiated nickel and cobalt-plated nickel wires were prepared as discussed previously. Polarization plots illustrating cell performance at 400° C. using various anode compositions are shown in FIG. 8 . The general performance increased in the order of corrosion resistance, in the order of nickel, Monel®, lithiated nickel, and cobalt-plated nickel. Each electrode type except the lithiated nickel was observed to have a matte black film after use, which was likely a mixed layer of nickel oxides (or cobalt oxide, as appropriate). This indicates that the mixed layer is a stable, protective oxide film that protects the anode from corrosion. The lithiated nickel electrode remained dark gray in color. Since the anodic treatment process for this anode created a surface film prior to its use in the cell, it is likely that this layer protected the underlying metal and prevented any further oxidation and discoloration.
[0032] The Monel® anode exhibited significantly less polarization than the pure nickel, which is somewhat surprising due to the fact that Monel® is an alloy with a high percentage of nickel. It is likely that any increased performance of the cell using a Monel® anode relative to nickel could be due to increased electrode surface area rather than simply an improvement in surface conductivity. Copper oxides are not stable in hot hydroxide environments, and in fact strong hydroxide solutions are often used in the electronics industry as a soldering flux. The result may be a surface de-alloying of the Monel®, producing a higher surface area nickel oxide relative to that forming on the pure nickel anode.
[0033] The lowest amount of electrode polarization was observed with the cobalt-plated nickel anode, although its performance lies quite close to that of the lithiated nickel anode. The oxides covering the surfaces of both of these electrodes probably created a significantly lower electrical resistance barrier in the anode region of the cell.
[0034] The United States Department of Energy Office of Energy Efficiency and Renewable Energy (EERE) has specified cost targets for the production of hydrogen in order to ensure the cost-competitiveness of hydrogen fuel in relation to other available fuels. For example, in order to make hydrogen a competitive fuel alternative to gasoline in the light-duty vehicle market, hydrogen must be produced for a cost of less than three dollars per kilogram (one kilogram of hydrogen contains approximately the same energy content as one gallon of gasoline). For electrolyzer applications, the cost of hydrogen generation is largely determined by the cost of the electrical power used. For example, a typical room temperature and pressure alkaline electrolysis unit may operate with a cell potential of 1.8 V and a thermal efficiency of 80%, using electricity at an off-peak price of 7.5 ¢/k Wh to produce hydrogen at an electrical cost of about $4.50/kg. If the cell potential is reduced to 600 mV under conditions of elevated pressure and temperature, as is possible with the invention described here, the electrical cost of hydrogen production drops to $1.50/kg, well below the EERE production cost goal of $3/kg of hydrogen.
[0035] While the invention has been illustrated and described in detail in the drawings and foregoing description, the same is to be considered as illustrative and not restrictive in character. Only certain embodiments have been shown and described, and all changes, equivalents, and modifications that come within the spirit of the invention described herein are desired to be protected. Any experiments, experimental examples, or experimental results provided herein are intended to be illustrative of the present invention and should not be considered limiting or restrictive with regard to the invention scope. Further, any theory, mechanism of operation, proof, or finding stated herein is meant to further enhance understanding of the present invention and is not intended to limit the present invention in any way to such theory, mechanism of operation, proof, or finding.
[0036] Thus, the specifics of this description and the attached drawings should not be interpreted to limit the scope of this invention to the specifics thereof. Rather, the scope of this invention should be evaluated with reference to the claims appended hereto. In reading the claims it is intended that when words such as “a”, “an”, “at least one”, and “at least a portion” are used there is no intention to limit the claims to only one item unless specifically stated to the contrary in the claims. Further, when the language “at least a portion” and/or “a portion” is used, the claims may include a portion and/or the entire items unless specifically stated to the contrary. Likewise, where the term “input” or “output” is used in connection with an electric device or fluid processing unit, it should be understood to comprehend singular or plural and one or more signal channels or fluid lines as appropriate in the context. Finally, all publications, patents, and patent applications cited in this specification are herein incorporated by reference to the extent not inconsistent with the present disclosure as if each were specifically and individually indicated to be incorporated by reference and set forth in its entirety herein. | A method and apparatus for dissociating water. A reaction chamber contains an anode and a cathode submerged in an aqueous hydroxide electrolyte. The temperature of the aqueous hydroxide electrolyte in the reaction chamber is elevated to least 280° C. The pressure of the aqueous hydroxide electrolyte in the reaction chamber is likewise elevated to least 2 atmospheres. An electrical voltage is applied across the anode and cathode using an electrical power supply and oxygen and hydrogen are formed from the water contained in the aqueous hydroxide electrolyte. | 2 |
This is a continuation-in-part of application Ser. No. 12/284,559 filed Sep. 23, 2008. Application Ser. No. 12/284,559 is hereby incorporated by reference in its entirety.
BACKGROUND
Field of the Invention
The present invention relates generally to lighting and more particularly to an energy savings under-cabinet lighting system having a USB port and using Light Emitting Diodes (LED's).
Description of the Problem
There is a need for saving more energy in these under-cabinet luminaries using specifically designed integral power supply with low power consumption to provide power to the Energy Saving LED's. This invention is an energy saving under-cabinet lighting system.
A light emitting diode (LED) is a semiconductor device that creates light using solid-state electronics A diode is composed of a layer of electron nch material separated by a layer of electron deficient material which forms a junction Power applied to this junction excites the electrons in the electron rich material leading to photon emission and the creation of light. Depending on the chemical composition of the semiconductor layers, the color of light emission will vary within the visible range of electromagnetic spectrum.
LED's are much more energy efficient than their incandescent and fluorescent lamps LED's are very energy efficient producing up to 90 percent light output with very little heat dissipation. Also, LED lighting technology includes features such as less energy consumption, long service life, high quality light, and suitability for cold temperature operation In addition, LED's do not contain mercury and are environment friendly
In addition, there is a great need to place a USB port on the surface of lighting fixtures to charge accessories such as laptops, tables and cellular telephones. However, charging lithium-ion batteries has fire hazard problems in that, if they receive too much charging current, they overheat. It would be very advantageous to have a lighting system with a USB port that can safely charge accessories without the danger of overheating.
Generally there are 2 types of power supplies, magnetic and electronic switch mode In this lighting system, the switch mode electronic power supply is used for energy efficiency, low profile, and light weight, to provide power to LED's.
SUMMARY OF THE INVENTION
The present invention relates to an energy saving under-cabinet luminaries using an energy efficient switch mode power supply optimized to provide maximum power to the LEDs while remaining within UL class 2 requirements of the Power Supply. These luminaries have a safe USB charging port that can safely charge lithium-ion batteries of accessories.
The present invention provides an energy saving under-cabinet Luminaire consisting of an enclosure, Class 2 integral power supply to provide power LEDs arranged in a special pattern to effectively replace 8 W, 13 W and 15 W fluorescent lamps or equivalent halogen lamps resulting in 50% of energy savings. Every component is individually optimized to save energy. The simplicity of the power supply using very few components greatly improves the reliability of this lighting system. The power supply is isolated and coupled to the LEDs so that it has a power factor of at least 90%.
A specially angled diffuser to converge the light output from the lighting system of the working area of the under-cabinet. The lenses of the LEDs are so chosen that the inner array near the wall has 30 degrees spread, and the outer array away from the wall has 60 degree spread to achieve more light in the working area of the under-cabinet.
DESCRIPTION OF THE FIGURES
Attention is directed to several figures that illustrate features of the present invention:
FIG. 1 shows the full exploded view of the entire LED under-cabinet unit lamp unit with all components marked.
FIG. 2A shows the front view of a first type of quick input connector for easy electrical connections.
FIG. 2B shows the front view of a second type of quick output connector for easy electrical connections.
FIG. 3A shows the front view array of layout of the LED's on a printed wiring board for 56 LED boards.
FIG. 3B shows the front view array of layout of the LED's on a printed wiring board for 80 LED boards.
FIG. 4 shows the wiring of 80 LED's in series parallel circuit.
FIG. 5 shows the wiring of 56 LED's in series parallel circuit.
FIG. 6 shows the schematic diagram of the circuit of the LED Power Supply with components marked.
FIG. 7 shows the construction details of the output transformer of the LED Power Supply.
FIG. 8 shows a view of the LED under-cabinet unit lamp unit with a USB port.
FIG. 9 is a schematic diagram of a power supply for the USB port with a safe charging feature.
Several drawings and illustrations have been presented to aid in understanding the present invention. The scope of the present invention is not limited to what is shown in the figures.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the preferred embodiment, as illustrated in FIG. 1 , the main components are the input power connector 8 , coupled to an external power cord 9 , an enclosed SMPS power supply 3 , providing the necessary voltage and content current to the LED's 6 , a simple resistive dimmer potentiometer switch 2 , to reduce the current to the LED's to create dimming effect, a main on/off switch 4 , and an output connector 5 to link the unit with an external interconnect cord 10 to another unit.
The unit can be used with quick connectors for electrical safety. FIG. 2A shows the front view of a first type of quick input connector for easy electrical connections, while FIG. 2B shows the front view of a second type of quick output connector. The connector in FIG. 2A has a round/square configuration, while the connector in FIG. 2B has a round/round configuration.
Two LED configurations can be used, the first with 56 LEDs and the second with 80 LED's. The 56 LEDs put out enough light output to replace an under-cabinet light fixture using one F8T5 (8 W) fluorescent lamp or equivalent lamp. This is shown in FIG. 3A . The 80 LEDs put out enough light output to replace and under-cabinet fixture using one F15T8 (15 W) or F13T5 (13 W) fluorescent lamp as shown in FIG. 3B . The numbers 56 and 80 are chosen to be cost effective. These numbers can change depending on growth of LED technology resulting in cost reduction by using fewer LED's with higher lumens per watt. FIG. 4 shows a schematic of the 80 LED circuit, while FIG. 5 shows a schematic of the 56 LED circuit. In each case, there is a current-limiting resistor 13 in series with the array and a capacitor 14 in parallel with it.
The design of the power supply is so chosen to put out 30 VDC maximum and still come under Class 2 requirements of Underwriters Lab (UL Inc.) Standard 1310 by limiting the voltage and current for safety considerations without compromising the optimum performance. An embodiment of such a class 2 power supply is schematically illustrated in FIG. 6 .
The first stage of power supply has an input stage filter network consisting of a metal oxide varistor 17 , rated at 150V for surge suppression, a safety current limiting fuse 27 rated ½ A 250 VAC, and an across-the-line capacitor 6 , rated 22 pF at 250V to absorb the transients.
The second stage is a full wave bridge rectifier consisting of a bridge rectifier 18 , with four diodes, rated 1 Amp. 400V with a filter capacitor 20 , rated 4.7 uF, 400V.
The third stage is a is a feeder network coupling the rectified AC voltage to an integrated control chip 21 which determines the pulse width after converting the rectified voltage to a high frequency chopped voltage.
The processed signal is fed to the transformer 26 with a ferrite core having the following construction:
Primary Windings:
Wind 18T on the magnet core EFDI5 FROM Pin I to Pin 3 by 0.15 enamel.
Secondary Windings:
Wind 135T on the magnet core EFDI5 FROM Pin 2 to Pin 4 by 0.2 mm enamel.
Wind 32T on the magnet core EFDI5 FROM Pin 8 to Pin 5 by 0.2 mm×3 enamel.
An auxiliary secondary has 7 turns of 0.15 mm enameled copper wire. This winding is also used in the feed back circuit to regulate the output voltage and current.
The transformer 26 steps down the input high voltage pulses to low voltage pulses. The diode 28 , rated 1 Amp. 400V is a rectifier which is coupled to a resistor 32 rated 5.1 ohms through inductor 29 .
An output filter network consists of a resistor 34 rated 10 Ohms coupled to a capacitor 35 rated 680 pF 150V in series coupled to parallel capacitors 36 and 39 rated 220 uF 50V to smooth out the ripple in the output waveform. Output filter choke 29 is coupled between capacitor 37 and diode 28 . This choke stores magnetic energy to provide a constant output current and voltage to LED's.
Resistor 38 rated 44 k ohms ½ w, is connected to choke 29 . Choke 29 and a parallel capacitor 33 rated 470 uF 30V form the output filter network.
An adjustable reference zener diode 30 is provided to regulate output voltage and current. This zener is coupled to the power supply through resistors 32 and 38 , rated 5.1 k Ohms and 44 k ohms respectively.
The turn on reference voltage is determined by resistors 32 and 38 . When the output exceeds the set voltage, the zener diode 30 provides a turn on signal to opto-isolator 40 , model PC8 17 which is coupled to capacitor 23 rated 22 pF 50V which is further coupled to pin 5 of 21 to regulate the output. Capacitor 22 rated 68 pF 50V provides the timing frequency for oscillations.
Diode 24 rated 1 Amp. 700V is coupled to the transformer auxiliary winding of transformer 26 and capacitor 25 rated 47 uF 16 V. This network provides start up current for the transformer oscillations. Capacitor 37 rated 100 uF 50 V provides necessary filtering of the output voltage by reducing the output ripple.
The LED's are laid out in a Flame retardant Printed Wiring Board (PWB) as shown in FIGS. 3A and 3B and convert the electric power input into visible white light to illuminate the under-cabinet area. The output coupling connector 10 shown in FIG. 1 may be used to couple another unit as needed.
FIG. 7 is an illustration of output transformer segments, primary 41 , auxiliary winding 42 and secondary 43 .
FIG. 8 shows a view of a fixture with a USB port 50 . The USB port is conveniently located for safe charging of accessories. The present invention can also be equipped with a polycarbonate plastic diffuser 51 shown in FIG. 8 that is about 2 mm thick of the type of translucent plastic called LEXAN™ made by General Electric and others. This diffuser is used for dispersion of dots pixualization from the LED in order to obtain uniform lighting. This reduces the Dot Matrix LED lighting. The optimum distance from the LEDs to the diffuser has been found to be 17 mm which makes the light more uniform and greatly reduces the pixualization further reducing the Dot Matrix LED lighting.
FIG. 9 shows a schematic diagram of an embodiment for a USB port power supply: The 120V, 60 Hz power from the mains has input fusible resistors R 1 rated 1 ohm, 1 watt. It is then rectified by a bridge rectifier Dl. The rectified signal is filtered by a capacitor C 2 rated 6.8 uF 400V. The filter network is π (PI) filter formed by C 1 , R 1 and C 4 and further filtered by choke L 1 and capacitor C 2 . These filters also help to reduce Electro Magnetic Radiation (EMI) back to the input mains by conduction process. The filtered output is coupled to a ferrite core high frequency transformer T 1 . The transformer is further coupled to Control IC chip U 1 . This controls the pulse width and frequency of rectified waves of the Primary of transformer T 1 .
There is a feed winding (pins 4 and 5) set up through a potential divider circuit formed by resistors R 6 and R 7 that is coupled to chip U 1 . This controls the output voltage constant 5 VDC by controlling the pulse width. The secondary of the transformer (pins 6 and 10) is stepped down low voltage pulses and further smoothly rectified by a diode D 8 rated 2 Amp 50 V. This signal is then fed to a capacitor C 51 further smoothes the ripple and coupled to capacitor C 52 through a series filter inductor choke L 10 . Across the output terminals pin 1 and pin 4 an indicator LED is connected in parallel with a series current limiting resistor R 56 rated 470 Ohms ½ W. The output voltage is a regulated 5 VDC.
The 5 VDC output is connected to pins 1 and 4 of the USB connector (outer pins). The output pin 1 is connected to a series positive temperature coefficient (PTC) thermistor to regulate and limit the charging current to a safe value of approximately 400 mA. Excessive charging current will result in overheating the lithium-ion batteries resulting in a fire hazard. The lithium-ion batteries have a very high charge density. So, charging current should be limited to safe value between 300-400 mA for typical charging a laptop or a cellphone. The PTC thermistor PT 1 typically offers less than 1 ohm under operating normal current and the Resistor value increases to very high value to limit the charging current
The thermistor PT 1 is operated under self heating mode. In this mode, it is in series connected with the battery load. It heats up as the current increases until it reaches a critical temperature Tc; then the resistance increases by large amount thereby reducing the current. So it acts as safe cut off regulator reducing the hazard created by excessive charging current to the battery.
The Thermistor PT 1 is so chosen in such a way that the typical resistance is approximately 0.3 ohm at 25 degrees C. at non-trip current (Int), and the value increases to 1-2 k Ohms or more at around 450 mA at trip current (It). This feature of the present invention positively prevents the batteries in the charging accessory from overheating by providing over-current protection.
The 5 VDC output is voltage is further divided to approximately to 2.5 VDC by potential dividers formed by resistors R 52 and R 54 , rated 10 k Ohms ½ w which couples to pin 2 of the USB Port. Resistors R 53 rated 10 k Ohm ½ W and R 55 rated 10 k Ohm ½ W form another potential divider that couples to pin 3 of the USB port. In this embodiment of the power supply, the pins do not transfer any data since no data is stored or delivered by the under-cabinet luminaire.
The power supply from the mains 120 VAC 60 Hz, can also be connected to the convenient outlet.
Several descriptions and illustrations have been presented to aid in understanding the present invention. One with skill in the art will realize that numerous changes and variations may be made without departing from the spirit of the invention. Each of these changes and variations is within the scope of the present invention. | An energy efficient under-cabinet lighting system with a low profile switch mode power supply complying with Class 2 requirements. This power source is enclosed in a container to provide constant current to an array of light emitting diodes LEDs that are characterized by long life and low power usage. The system is designed to replace existing under-cabinet fluorescent lamp fixtures. A diffuser minimizes pixelization. The unit is also equipped with a safe-charge USB port that can safely charge lithium-ion batteries of accessories like tablets and cellphones with no danger of overheating their batteries. | 5 |
BRIEF DESCRIPTION OF THE INVENTION
1. Field of the Invention
This invention relates to tools arranged with a conventional drill string for reaming well bores to a desired diameter during or after drilling of that well bore.
2. Prior Art
Under reamers useful for expanding well bores have long been in common use and it has been common to provide such tools with cutting members that are designed to be moved or extended against a well bore wall after the tool is positioned within the well bore, for turning through a conventional drill string to effect a desired widening of all or sections of the well bore. An example of one such under reaming tool is shown in a U.S. Pat. No. 1,739,823. The device of this patent involves mechanically controlled cutting elements that are operated through a drill string, and are capable of being extended and retracted by an operator on the surface.
Another example of an under reamer tool for arrangement within a conventional drill string is shown in a U.S. Pat. No. 2,809,015. The tool of this patent also involves mechanically moved and controlled cutting elements for movement into engagement with a well bore wall, which movement is effected by a compression of the tool as by appropriate unlocking thereof and forcing the drill string downward to extend outwardly the cutting elements thereof.
Unlike the above-cited mechanically operated reaming tools, the present invention does not involve any direct linkage, either mechanical or electrical, through the drill string to the surface to command or effect the extension or retraction of cutter portions of cutting elements thereof. The cutters of the present invention are moved outwardly by centrifugal force as when the drill string and present invention are turned, until a cutting edge of each cutter portion contacts and is thereafter drawn into the wall of the well bore with retracting of the individual cutters being effected with the drill string stationary and whereafter it and the tool are lifted from the well bore. The edge of each cutter, should it contact the well bore wall, or a shoe, or a first diameter reduction of casing therein, or the like, being urged into a retracted attitude or position within the tool body; the under reamer tool of the present invention, therefore, being different in both construction and operation from the above-cited prior art devices.
An additional example of an under reamer tool for use in a drill string that is operated by fluid pressure is shown in U.S. Pat. No. 3,556,233, which patent, as per the above discussion, is also unlike the under reamer tool of the present invention.
Within the knowledge of the inventor, the under reamer of the present invention is unlike in its construction or use any machine or device known for enlarging a well bore.
SUMMARY OF THE INVENTION
It is a principal object of the present invention to provide an under reamer tool for arrangement in a conventional drill string, the tool involving movable cutting elements that are capable of extension from and retraction to within the tool body for enlarging a well bore with extension and retraction thereof being controlled only by turning the drill string and pulling that drill string from the well bore.
Another object of the present invention is to provide an under reamer tool capable of being inserted through a pipe or liner arranged within a well bore, which tool will, under the impetus of centrifugal force when the drill string connected thereto is turned, extend cutters thereof into engagement with the well bore wall immediately below that pipe to ream away materials therebelow so that the pipe can be further inserted into that well bore, but will retract into the tool body, allowing the tool to be withdrawn through that pipe when the drill string is lifted from the well bore.
Another object of the present invention is to provide an under reamer tool for installation in a conventional drill string immediately above a conventional bit arrangement whereby the turning of the drill string turns also the under reamer tool to widen out the well bore as that well is being drilled.
Still another object of the present invention is to provide an under reamer tool having cutters thereof that are journaled or arranged on appropriate journaled units to travel within the tool body under the impetus of centrifugal force to extend therefrom to engage the wall of a well bore wherein the tool is turned, which cutters will retract back into the tool body when the tool is not turned and should the top of a cutter contact an object such as the well bore wall, or a shoe, first diameter reduction, or the like, of a pipe or liner therein when said tool and connected drill string are withdrawn from the well bore.
Still another object of the present invention is to provide an under reamer tool that is simple to construct with all movable elements thereof being arranged so as to be independent from direct control or linked to the well bore surface other than through the drill string connection to the tool, cutters of the tool being extended under the impetus of centrifugal force when the tool and drill string are turned, the cutters being drawn into the wall of a well bore to uniformly enlarge that well bore when they are moved outwardly to contact therewith, which cutters will retract automatically as the drill string is lifted from the well bore, and when the top edge of each cutter contacts the wall of a well bore, a shoe, first diameter reduction, or the like, or a pipe therein, the cutter will be urged to a retracted attitude within the tool body, the area within the tool body within which the cutter is retracted being arranged to receive a continuous fluid purge during turning of the drill string.
Briefly stated, the present invention comprises an under reamer tool for appropriate connection in a conventional drill string above a bit, the tool of the present invention being turned by that drill string, as is the bit, to enlarge all or part of a well bore to a desired diameter. The tool of the present invention includes a cylindrical body formed from steel or the like, that has a plurality of elongated transverse openings formed therein that contain aslant shafts or crosshead guides on which shafts or guides are journaled cutters or crossheads mounting cutters. The aslant attitude of the individual shaft or crosshead guide is such that it forms an angle outwardly from the body longitudinal center to the well bore wall such that the individual cutter will make an optimum cutting angle for intrusion into the well bore wall and will be drawn into the wall when an edge thereof first contacts that wall, with retraction of the individual cutter or crosshead and mounted cutter occurring when the drill string is pulled from the well bore and a top edge of each such cutter contacts the well bore wall, a shoe, or end of a well bore liner, or the like, with the cutter thereby being urged back along the shaft or crosshead track into a recessed attitude within the tool body.
The preferred cutter has arranged, as the cutting and well bore wall engaging surface, a flat or somewhat rounded cutting surface that is capable of reaming away to a flat surface, the well bore wall. Such cutter preferably has a cone shape and incorporates appropriate roller bearings that are arranged in a center longitudinal hole therethrough, journaling the individual cutter onto the shaft or onto a post of the crosshead. The individual cutter also incorporating at least one thrust bearing therewith to absorb forces generated when the cutter cuts into the well bore wall.
The under reamer tool of the present invention also incorporates an appropriate threaded shaft or stem on one end thereof for attaching it to a drill string and an appropriate threaded collar or recess therein for coupling a conventional bit thereto. Further, within the tool body are arranged purge ports that intersect a longitudinal fluid flow passage that passes through the tool body and into the bit therebelow, which purge ports will pass liquid therethrough to continuously scour out materials from the within area of the tool body that houses the cutters or crossheads therein when said cutters or crossheads are moved into a stowed attitude.
Further objects and features of the present invention will become apparent from the following detailed description, taken together with the accompanying drawings.
THE DRAWINGS
FIG. 1 is a side elevation view of an under reamer tool of the present invention shown arranged within a well bore attached to a drill string, the tool having a conventional drill bit attached to its lower end, showing also portions thereof broken away to expose portions of the tool interior;
FIG. 2, a top plan sectional view taken along a line 2--2 of FIG. 1, showing a first preferred embodiment of the tool's arrangement of cutting elements, each having cutters thereof extended into the wall of the well bore as when the tool is operated to enlarge a well bore;
FIG. 3, an exploded sectional view taken within the line 3--3 of FIG. 1, showing a cutting element as consisting of a cutter that is journaled onto a shaft to slide up and down thereon, that cutter as shown in broken lines, is being moved to a stowed attitude within the tool body;
FIG. 4, a sectional view of a second embodiment of a cutting element that should be taken as preferably being incorporated with the tool of FIG. 1, and involves a cutter that is journaled to a crosshead that is arranged to travel on a crosshead guide, the crosshead in broken lines, shown as having been moved to a recessed attitutde within the tool body; and
FIG. 5, a top plan sectional view taken along the line 5--5 of FIG. 4, showing a post portion of the crosshead whereon the cutter is journaled, the crosshead shown arranged on the crosshead guide that is secured to the tool body.
DETAILED DESCRIPTION
Referring now to the drawings:
In FIG. 1 is shown a preferred embodiment of an under reamer tool 10 of the present invention, hereinafter referred to as a tool, that is shown connected at a threaded neck portion 11 thereof, to the end of a conventional drill string 12 that is shown in broken lines. Attached at a threaded collar or recess 15 within tool 10 opposite to neck 11 is shown a conventional drill bit 13 having a threaded shank portion 13a that is turned appropriately into the threaded collar or recess 15 formed within a cylindrical body 14 of tool 10. The tool 10 and a portion of drill bit 13 are shown in FIG. 1 in cross section as being arranged within a conventional well bore 16, the drill bit turned therein to form a bore whose diameter is reflective of its cross section configuration, the following tool 10 enlarging that bore to the desired diameter so that a pipe or liner 17 can be installed therein. Shown in FIG. 1, the liner 17 has a shoe 18 arranged on its lower end which shoe has an inner lip 18a formed thereon that is appropriately slanted inwardly away from the shoe end to accomodate a cutter 23 of the tool 10 passing thereby the function of which cutter will be explained in detail later herein.
Shown in FIGS. 1 and 2, the tool body 14 is essentially a solid unit having, as has been described, a neck 11 arranged on one end with a recess or collar 15 formed in the other. Further, the tool body 14, as shown best in FIG. 2, has flutes 19 formed therein on 120° centers that are semi-circular in shape, which flutes 19 open to the outer wall of tool body 14 to accommodate cutting elements 20 housed therein whose function will be explained in detail later herein. While these flutes 19 are shown in FIG. 2 as being preferred, it should be obvious that tool 10 could incorporate more than three such flutes, which flutes also could be of a different shape than is shown without departing from the subject matter coming within the scope of this disclosure. While not shown, to facilitate manufacture of tool body 14, it may be most expedient to manufacture the tool body in sections, cutting flutes 19 from a center portion and thereafter joining appropriately top and bottom portions thereof to that fluted center portion to form tool body 14.
As shown best in FIGS. 1 and 2, tool body 14 has a longitudinal passage 21 formed therethrough for receiving mud, fluid or the like from the drill string 12 and passing it therethrough and into the drill bit 13. Further, the tool body has lateral ports 22, shown best in FIG. 1, that extend outwardly, at normal angles, from passage 21 to intersect individual flutes 19 for providing for fluid passage therethrough to scour and purge away materials, such as soil, rock chips, or the like, from within that fluted area for facilitating operation of the cutting element 20 arranged therein, particularly retraction thereof, to within the tool body 14 as will be explained later herein.
In FIG. 3 is shown a first preferred embodiment of a cutting element 20 arranged in a flute 19 within the tool body 14 with ports 22 shown therein as intersecting flute 19 to pass air or fluid therethrough to clean and scour both the flute 19 and the cutting element 20 itself. The cutting element 20 shown therein perferably involves a cone-shaped cutter 23 that has a center longitudinal bore 24 formed therethrough and has preferably diamond chips or pieces of other cutting or abrasive surfaces 25 secured around the cone outer surface. Bearings 26 are arranged within the the longitudinal bore 24 journaling the cutter 23 to a shaft 28, and a thrust bearing 27 is secured across the longitudinal bore 24 on the top of cutter 23 whose function will be explained later herein. The shaft 28 onto which the cutter 23 is journaled is arranged in an aslant attitude across the flute 19, that shaft initially being turned through an opening 29 that is formed through the tool body 14 outer wall, passing across the flute 19 and its end 28a is turned into another hole 30, formed also in the tool body 14. Hole 30 is threaded at 31 as is hole 29 threaded at 29a to receive threads formed in shaft 28a and in the top thereof at 28b. A notch 28c is formed across the top end of shaft 28 for receiving a screwdriver blade, or the like, not shown, to turn that shaft appropriately through hole 27 and into hole 30. So arranged, the cutter 23 is free to slide up and down on shaft 28, turning freely thereon around bearings 26, which bearings 26 along with thrust bearing 27 are preferably ball bearings, though other type bearings could conceivably be used for minimizing friction of the cutter 23 when it is turned or moved along shaft 28.
During operation of tool 10, as described hereinabove, cutter 23 is journaled to rotate on shaft 28 and is also arranged to travel vertically thereon. In FIG. 3 the cutter 23 is shown in its extended attitude whereat it will engage and cut, along a flattened outer edge 23a thereof, the wall of well bore 16, to form a flattened portion 16a with a slanted portion 23b of the cutter 23 engaging and forming at 16b a slanted wall portion. So arranged, with the cutter 23 in the attitude shown in FIG. 3, the well bore 16 is first formed by bit 13 and is then enlarged to a desired diameter by cutter 23, the cutter 23 first enlarging that well bore by the action of the cutter slanted portion 23b and finishing that cut to a smooth wall by action of the flattened outer edge 23a thereof. In operation, when a corner 23c of cutter 23 between the slanted portion and flattened outer edge 23a and 23b or the flattened outer edge 23a thereof first engages well bore wall, as by turning tool 10 through drill string 12, the cutter being urged outwardly by centrifugal force, the cutter will be caught in that wall and will be pulled therein to its extended attitude as shown in FIG. 3. In this attitude cutter 23 turns freely on bearings 26 and against thrust bearing 27, which thrust bearing 27 is either mounted in tool body 14, adjacent to the top of cutter 23 or is mounted in the cutter itself to engage the tool body at 14a. So arranged, a minimal friction load occurs between the cutter 23, shaft 28, and tool body at 14a, when the cutter reams the well bore wall as is shown in FIG. 1.
During boring of well bore 16, the cutter 23 is in the attitude shown in FIG. 3, increasing the diameter of that well bore by shaving away the wall thereof to a desired diameter. Thereafter, to remove the drill string 12, connected tool 10, and drill bit 13 from the well bore 16, it is necessary only to discontinue turning of the drill string and to lift it and the connected tool and drill bit from the well bore. During this procedure, when and if the cutter 23 contacts, proximate to its edge 23d, any obstruction or the lower end of liner 18, that contact will urge the cutter to slide down shaft 28 to the attitude shown by broken lines in FIG. 3. In this attitude the cutter flat surface 23a is contained within tool body 14 and that tool body will pass freely up within liner 18 to the surface. Shown best in FIG. 1, to facilitate this inward sliding of cutter 23 on the aslant shaft 28, the liner shoe end at 18a is preferably slanted so as to prohibit cutter 23 from binding thereagainst and possibly damaging the cutter or pulling the liner from the well bore.
It should be noted that the tool body 14 and cutting element 20 can all be manufactured from standard materials for constructing drill bits, cutters, and the like, by standard manufacturing techniques common to the drilling tools manufacturing industry. During such manufacture, particularly the removal of flutes 19 and forming of holes 29 and 30 therein, conventional manufacturing methods and techniques are preferably employed and, if necessary to facilitate such manufacture and to keep costs of manufacture at minimal expense, the tool body 14 can be manufactured in sections as mentioned hereinabove and, thence, joined appropriately into the tool body shown without departing from the subject matter coming within the scope of this disclosure.
In FIG. 4 is shown another embodiment of a cutting element 40 for use in tool 10 for operation as has been described with respect to cutting element 20. It should, therefore, be understood that cutting element 40 performs the same function in essentially the same manner as does the above described cutting element 20 with the distinction between the two cutting elements being that each cutting element 40 involves a crosshead 42 whereon a cutter 46 is journaled, that crosshead being arranged to slide freely up and down on a crosshead guide 41 that is arranged in an aslant attitude in flute 19 of tool body 14. Shown in FIGS. 4 and 5, the crosshead guide 41 has fitted, in sliding arrangement thereover, a track 42a of the crosshead arranged to travel freely thereover. Also, the crosshead has a hole 43 formed therethrough through which hole a post 44, shown in FIGS. 4 and 5, is installed and maintained by a nut 45, said post preferably being parallel to the walls of the crosshead guide 41 and track 42a. Post 44, as shown best in FIG. 4, preferably has a larger diameter end at 44a for installation through hole 43 in crosshead 42, which hole 43 is tapered appropriately such that post end 44a just fits therein, and is reduced therefrom at its opposite end. Over post end 44b is shown installed cutter 46, a center longitudinal opening 46a formed therethrough fitting over post end 44b. Along the post opposite end 44b, within the center longitudinal opening 46a, are arranged bearings 47, that are preferably ball bearings, but could, of course, be bushings, or the like, with a thrust bearing 48, that is also preferably a ball bearing but could likewise be a bushing, shown sandwiched between the bottom surface of cutter 46 to ride on the top 42b of a crosshead 42. The cutter 46 is maintained on post opposite end 44b by turning a nut 50 thereover, which nut 50 rides against a washer 49 that extends across the top of opening 46a formed through cutter 46. So arranged, cutter 46 is journaled by bearing 47 onto post opposite end 44b to turn freely thereon with the thrust bearing 48 dissipating forces encountered that tend to bind the cutter 46 against the top 42b of crossarm 42.
Operation of the cutting element 40, it should be understood, is like or similar to that described with respect to cutting element 20, excepting cutter 46 does not move vertically, rather the crossarm 42 on which it is journaled moves vertically. When the tool 10 mounting cutting element 40 is turned, the crosshead 42 will move along the aslant crosshead guide 41, traveling upwardly under the impetus of centrifugal force and will be moved downwardly when the tool is not turned and when a top edge 46b of cutter 46 engages and is pushed downward by the wall of the well bore or shoe end of a pipe or liner arranged within that well bore similar to the movement of the described cutter 23 after the drill string attached thereto has ceased turning. When the top edge 46b of cutter 46 so engages an obstruction within the well bore, it will, in turn, force crosshead 42 along crosshead guide 41 to the attitude shown by broken lines in FIG. 4, in which attitude the cutting element 40 is stored within the tool body 14 allowing for the tool body 14, drill string and drill bit attached thereto to be withdrawn from the well bore.
Hereinabove, the present invention in a tool 10 has been described as having two preferred embodiments of cutting elements 20 and 40 that each operate essentially in the same manner in that they are arranged to be urged outwardly when tool 10 is turned by a conventional drill string attached thereto, such that edges of cutters thereof contact and are drawn into the wall of a well bore so as to enlarge the diameter thereof to a desired configuration. Retraction of the cutters of these two cutting element embodiments is effected to reposition the cutters within the body of the tool by ceasing to turn the tool and by drawing it upwardly until an edge of the cutter thereof engages an obstruction, either in the wall of the well bore or the shoe end of a pipe or liner therein, with that contact encouraging the cutter to travel back into a recessed storage area within the tool body. The present invention, therefore, involves a cutting element having cutters arranged therewith that, when the tool is turned, will travel outwardly to engage the wall of a well bore and will cut that well bore to a desired configuration by turning of the tool only, which cutters will travel back into the tool to a recessed storage attitude for removal of the tool and connected drill string and drill bit from the well bore when the tool is not turned. Therefore, the present invention should not be limited to a particular configuration of cutting element or cutters therewith shown herein, but should be understood to encompass all cutting elements with cutters capable of traveling, under the urges of centrifugal force only, to engage a wall of a well bore, which cutters will be moved back into a retracted or stowed attitude within the tool body when centrifugal forces are removed therefrom and when the tool body thereof is lifted from the well bore.
While preferred embodiments of the cutting elements for the under reamer tool of the present invention have been shown and described herein, it should be understood that variations, changes, adaptations, modifications and the like may be made to the disclosed invention without departing from the subject coming within the scope and spirit of the following claims, which claims I regard as my invention. | The present invention consists of an under reamer tool for enlarging, scraping or smoothing a well bore. The tool is attached to a conventional drill string above a conventional bit and involves cutting elements that have retractable cutters arranged for extension from the tool to engage the well bore wall, each cutter, when the drill string is turned, being urged outwardly by centrifugal force until it engages the well bore wall, continued turning thereafter, pulling that cutter into its extended cutting attitude, reaming the wall to the desired diameter, cutter retraction involving ceasing turning the drill string and the pulling of the drill string and connected tool from the well bore. During that pulling should the cutter contact a shoe or first reduction of the well bore casing or the wall thereof, it will be urged into a stowed attitude recessed within the tool body, the under reamer tool of the present invention also incorporating scouring openings provided in the tool body opposite to the cutter storage areas to pass liquid or air therethrough from the drill string to purge and clean that area within the tool body, allowing the cutter to travel freely therein. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application claims the benefit of U.S. Provisional Patent Application No. 60/517,509, entitled “POOL,” which was filed Nov. 5, 2003, and U.S. Provisional Patent Application No. 60/533,184, entitled “POOL,” which was filed Dec. 30, 2003, the entire contents of each of which are hereby incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] The present invention relates to pools, especially larger pools typically referred to as swimming pools. However, the invention could be used to produce so-called swim spas, wading pools or the like.
[0003] A major breakthrough in pool construction occurred in about 1993, when Polynesian Pools, Inc. introduced the pool disclosed in U.S. Pat. No. 5,400,555. This is a so-called “vinyl liner” pool, in which the poolside walls are molded of high impact polystyrene. Each panel has top, bottom and end panel flanges, which can be secured to each other and to molded structural plastic braces projecting rearwardly from the wall panels. The fasteners for securing these components together comprise fasteners, each of which includes an elongated slot. One of the fasteners is integral with the pool brace, but other fasteners, while molded with the brace, are separable and are used as separate members. The integral peg protrudes through receiving apertures in the panel end flanges. The separate fasteners are passed through apertures in the brace and the panel end flanges. A peg having an inclined leading edge is then driven into the slot in the key to securely hold the abutting panels and the brace together. The slotted fasteners and pegs were made of nylon.
[0004] Others have since emulated this design. Some employ braces which project further away from the pool wall, i.e. a full two or three feet, in order to give greater support to a concrete or other deck placed above the braces around the perimeter of the pool. These wider braces are difficult to work with, however, since one normally does not want to have to “overdig” more than about two feet beyond the nominal edge of the pool where the walls are placed. If the braces extend two or three feet from the wall, one has to dig further at least in the area of the braces in order to accommodate the greater length.
SUMMARY OF THE INVENTION
[0005] The present invention comprises a wall and buttress construction for swimming pools in which deck support extensions can be secured to the top of the buttresses.
[0006] In another aspect of the invention, the wall includes a plurality of panels having end flanges at the sides of the panels, and a double slotted peg is provided. One of the slots is shorter to receive a wedge when a peg is placed through two abutting panel end flanges, and the other slot being longer to accommodate a wedge when the peg is being used to join a brace as well as two abutting end flanges.
[0007] Preferably the end flanges have elongated openings therethrough for receiving the pegs that are oriented diagonally, rather than either vertically or horizontally. They are much more easily visible/accessible for inserting pegs as a result of the diagonal orientation.
[0008] In another aspect of the invention, the wall panels themselves are reinforced with intersecting parabolic arches on the back surfaces thereof. In yet another aspect of the invention, the buttresses are provided with a plurality of plumbing saddles for receiving plumbing lines to plumb the swimming pool. In addition, the buttresses also preferably have oversized rebar holes, approximately three times the diameter of rebar, to make it easier to slide long lengths of rebar into the buttresses to facilitate anchoring the walls in the ground or in concrete footings.
[0009] These and other aspects, features and advantages of the invention will be more fully understood and appreciated by reference to the written specification and appended drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0010] FIG. 1 is a partially fragmentary perspective view of a pool according to one aspect of the present invention;
[0011] FIG. 2 is an exploded perspective view of a portion of the pool of FIG. 1 ;
[0012] FIG. 3 is a perspective view of a portion of the pool of FIG. 1 ;
[0013] FIG. 4 is a fragmentary, perspective view of a peg and wedge that may be utilized to interconnect adjacent panels of the pool;
[0014] FIG. 5 is a fragmentary view showing the peg and wedge in the assembled condition;
[0015] FIG. 6 is a plan view of the peg;
[0016] FIG. 7 is a plan view of the wedge;
[0017] FIG. 8 is a partially fragmentary, perspective view of a deck support extension;
[0018] FIG. 9 is a fragmentary, perspective view of a buttress and deck support;
[0019] FIG. 10 is a side view of a buttress and deck extension;
[0020] FIG. 10A is a fragmentary cross-sectional view of an upper portion of the pool wall;
[0021] FIG. 11 is a partially fragmentary, exploded perspective view of a buttress and optional tube into which concrete can be poured to provide additional support;
[0022] FIG. 12 is a fragmentary, perspective view of a buttress and anchor;
[0023] FIG. 13 is a perspective view of a portion of a pool and a buttress that includes leveling pads;
[0024] FIG. 14 is a perspective view of a first leveling pad having a first height;
[0025] FIG. 15 is a perspective view of a second leveling pad having a second height that is greater than the height of the first leveling pad of FIG. 14 ;
[0026] FIGS. 16A-16E are partially schematic views illustrating the different spacing heights that can be achieved utilizing the first and second leveling pads of FIGS. 14 and 15 ; and
[0027] FIG. 17 is a partially schematic view illustrating another leveling pad arrangement.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0028] For purposes of description herein, the terms “upper,” “lower,” “right,” “left,” “rear,” “front,” “vertical,” “horizontal,” and derivatives thereof shall relate to the invention as oriented in FIG. 1 . However, it is to be understood that the invention may assume various alternative orientations and step sequences, except where expressly specified to the contrary. It is also to be understood that the specific devices and processes illustrated in the attached drawings and described in the following specification are simply exemplary embodiments of the inventive concepts defined in the appended claims. Hence, specific dimensions and other physical characteristics relating to the embodiments disclosed herein are not to be considered as limiting, unless the claims expressly state otherwise.
[0029] With reference to FIG. 1 , pool 1 includes a plurality of panels 2 forming a wall 10 and a liner 3 . As described in more detail below, adjacent panels 2 can be quickly and easily interconnected utilizing pegs 25 and wedges 26 to form a strong and durable structure. The panels may be curved panels 4 having a relatively large or small radius, forming inside or outside corners. The panels 2 may include a cutout 5 that can be removed for installing a skimmer 6 . One or more buttresses 7 may be interconnected to the panels 2 to provide additional support. Also, a concrete deck 8 extends around the pool, and is supported by the buttresses 7 as described in more detail below. With reference to FIG. 2 , each panel 2 includes a wall 12 , an upper flange 13 , lower flange 14 , and vertically extending side flanges 15 . Parabolic ribs 16 and horizontal ribs 17 extend across the wall 12 to provide structural support. A circular rib 18 extends around a cutout 19 for mounting of a light (not shown). The panels 2 and buttress 7 are made of a polymer material having a tough outer skin and inner cellular structure providing a very strong and durable pool structure. Conventional coping 9 extends around the top edge of wall 10 and overlaps the joints formed at adjacent panels 2 to thereby reinforce the wall structure and align adjacent panels 2 . As also discussed in more detail below, coping 9 secures the upper edge 11 ( FIG. 10A ) of the pool liners to the panels 2 .
[0030] Each side flange 15 includes a plurality of openings 20 therethrough (see also FIGS. 3 and 4 ), and each buttress 7 includes a plurality of tabs or extensions 21 . Each tab 21 also has an opening 20 therethrough having the same shape, size, and orientation as openings 20 in flanges 15 of panels 2 . Openings 20 are in the form of an elongated slot having an enlarged center portion 20 . Slots 20 are preferably oriented at about a 45° angle relative to the vertical walls 12 of panels 2 . Pegs 25 extend through openings 20 , and a wedge 26 extends through a selected one of the openings 27 and 28 in wedge 25 to securely and tightly interconnect adjacent panels 2 . Alternately, conventional threaded nylon fasteners (not shown) may be inserted through the enlarged center portion 22 of openings 20 to interconnect the adjacent panels 2 .
[0031] If a pair of adjacent panels 2 are directly interconnected without a buttress 7 , the peg 25 is inserted through the openings 20 of the adjacent side flanges 15 of the panels 2 , until extension 29 contacts sidewall surface 30 ( FIG. 4 ) of side flange 15 . Wedge 26 is then inserted through the shorter opening 28 to interconnect the adjacent panels 2 . If a buttress 7 is to be interconnected to the panels 2 , the tabs 21 of the buttresses 7 are positioned adjacent the side surface 30 with the opening 20 of tab 21 in alignment with the openings 20 of the side flanges of the panels 2 . The peg 25 is then inserted through the openings 20 in the tabs 21 and side flanges 15 , and wedge 26 is inserted into the longer slot 27 in peg 25 . Thus, the different lengths of the slots 27 and 28 permit the peg 25 to be utilized for interconnecting adjacent panels 2 either with or without a buttress 7 . The side surface 31 of vertical flanges 15 of panels 2 are substantially smooth and uninterrupted, such that adjacent surfaces 31 abut one another when adjacent panels 2 are interconnected. The peg 25 and wedge 26 provide alignment for adjacent panels, such that additional alignment features are not required.
[0032] With further reference to FIG. 6 , peg 25 includes a central web portion 34 and a smoothly radiused thicker edge portion 35 that extends around the peg 25 to provide additional strength. Similarly, thicker radiused portions 36 extend around openings 28 to provide additional strength. Tapered surfaces 38 and 39 form a pointed end portion 37 of peg 25 . The tapered edges 38 and 39 facilitate insertion of the peg 25 in openings 20 , and also bring adjacent openings 20 into alignment during assembly. An end or head 40 distributes forces if a hammer or the like is used to tap or drive the peg 25 into openings 20 .
[0033] With further reference to FIG. 7 , wedge 26 includes a central web portion 41 and thicker, radiused edge portions 42 that provide additional strength. End 45 of wedge 26 includes a first tapered edge 43 and second tapered edge 44 . Edge portion 46 is tapered less than edge portion 44 , and provides a tight wedging action when wedge 26 is inserted into opening 27 or 28 of peg 25 . End or head 47 provides for distribution of forces if a hammer or the like is utilized to securely drive the wedge 26 into the opening 27 or 28 of peg 25 . Tapered edges 43 and 44 at end 45 facilitate insertion of wedge 26 and further contribute to quick and easy assembly of pool 1 . Edge 42 A may be serrated to provide a secure, high friction engagement with openings 27 , 28 of peg 25 to ensure that wedge 26 does not become dislodged. Wedge 26 is preferably inserted into slot 27 or 28 in peg 25 in the orientation shown in FIG. 4 , such that edge 46 contacts surface 30 of flange 15 . Alternately, wedge 26 may be installed in an orientation as illustrated in FIG. 5 , wherein serrated edge 42 A contacts surface 30 of flange 15 . The peg 25 and wedge 26 are made of a polycarbonate material that provides sufficient strength to structurally interconnect adjacent panels 2 and buttress 7 , and also provides impact resistance to prevent cracking during installation.
[0034] The peg 25 and wedge 26 provide for very quick and secure interconnection of adjacent panels 2 and buttresses 7 . Also, the angle of opening 20 ensures that the peg 25 and wedge 26 can be easily seen by the builder even if there is limited space between the wall 10 and the adjacent earth. Also, the wedge 26 tightly draws the adjacent panels 2 together. Side flanges 15 may be provided with five openings 20 including upper openings 20 A and 20 B ( FIG. 3 ), a central opening 20 C, and lower openings 20 D and 20 E. The upper and lower pairs of openings are spaced apart a distance “A”, and openings 20 B and 20 D are spaced a distance that is twice as great (“2A”). Tabs 21 of buttress 7 are also spaced such that openings 20 through tabs 21 of buttress 7 align with the openings 20 A, 20 B, 20 D and 20 E in side flanges 15 of panels 2 .
[0035] During assembly, a pair of adjacent panels 2 are positioned side-by-side, and a peg 25 is inserted through central openings 206 of the adjacent panels 2 . A wedge 26 is then inserted through smaller opening 28 of peg 25 . After the panels are interconnected at central openings 206 , a buttress 7 is positioned with tabs 21 adjacent a side flange 15 of one of the panels 2 , with opening 20 through tab 21 aligned with openings 20 of panels 2 . Pegs 25 are then inserted through openings 20 in tab 21 and flanges 15 , and a wedge 26 is then inserted in larger opening 27 to thereby interconnect the panels 2 and buttress 7 .
[0036] With further reference to FIGS. 8-10 , buttresses 7 include an outer vertical structural portion 49 , an inner vertical portion 51 , and inner structural portions 50 that extend at angles to form a structurally strong and rigid “X” configuration. As described in more detail below, upper horizontal structure 52 may provide support for a concrete deck 8 , and lower structure 53 provides for routing of plumbing. Upper portion of buttress 7 includes a pair of horizontally extending horizontal flanges 56 ( FIG. 8 ) forming a pair of horizontal slots 57 on opposite sides of buttress 7 . A deck support extension 54 has a generally flat C-shaped cross section. During assembly, extension 54 slides onto buttress 7 with end portions or flanges 58 of extension 54 received in slots 57 . Extension 54 is made of steel or other suitable material providing strength and durability. The deck support extension permits the concrete that is used to form deck 8 to be poured prior to compaction of soil 59 to provide for rapid construction of the pool. Buttresses 7 are preferably about 14 inches wide, and flanges 15 of panels 2 are about 4 inches wide. Extension 54 is about 30 inches long, such that a standard concrete deck 8 extends about 2 inches beyond end 54 A (see also FIG. 10 ) of extension 54 . The concrete material preferably extends downwardly around extension 54 and an upper part of buttress 7 . Rebar 64 may be positioned transversely on top of extensions 54 ( FIG. 9 ) such that it becomes embedded in the concrete deck 8 when the concrete is poured.
[0037] With reference to FIG. 10 , lower structure 53 of buttress 7 includes at least two plumbing cradles 60 that support pipes 61 (see also FIG. 1 ) for skimmer 6 , filters and/or other such components. As illustrated in FIG. 13 , buttress 7 may include three plumbing cradles 60 to support additional pipes or other lines. Rebar 64 (see also FIGS. 11 and 12 ) may extend through openings 62 and/or openings 63 in buttress 7 to provide additional structural support. The rebar 64 may also extend through a concrete footing 65 ( FIG. 10 ) to provide additional structural reinforcement. The lower portions of buttresses 7 are embedded in footing 65 to anchor and support the pool structure. A pair of extensions 67 slidably receive and retain a stake 66 that further secures and anchors the buttress 7 . Openings 68 (see also FIG. 3 ) in lower flange 14 of panels 2 receive a stake 69 that may be made from rebar to further anchor the panels 2 . As illustrated in FIG. 10A , coping 9 includes a channel that receives an enlarged, barbed edge 11 of lining 3 to thereby secure the liner 3 to the panels 2 . Self-tapping screws 77 attach coping 9 to upper flanges 78 of panel 2 . Coping 9 also provides a form/support for concrete deck 8 . Coping 9 is preferably made of a rigid corrosion resistant material such as aluminum.
[0038] With further reference to FIG. 11 , a polymer (e.g., PVC) or cardboard tube 70 may be used to form a concrete pilaster to support the deck 8 and buttress 7 . Tube 70 is first cut to the proper length, and a notch 71 is then cut into an upper edge 70 A of tube 70 . Buttress 7 includes a downwardly opening upper hook 100 (see also FIG. 8 ) and an upwardly opening lower hook 101 . During assembly, upper end 70 A of tube 70 is positioned adjacent outer surface 72 of buttress 7 , and tube 70 is shifted upwardly such that hook 100 is positioned in notch 71 . Lower end 70 B of tube 70 is then rotated inwardly towards buttress 7 , and tube 70 is then shifted downwardly until lower end 70 B engages lower hook 101 . Tube 70 is then rotated about its longitudinal axis to shift notch 71 away from upper hook 100 , thereby attaching tube 70 to buttress 7 . Concrete may then be poured into the tube 70 to form a pilaster that provides additional structural support for the deck 8 .
[0039] With further reference to FIG. 12 , a “deadman anchor” 73 may be secured to the buttress 7 by an adjusting rod 74 and conventional hardware 75 .
[0040] With further reference to FIG. 13 , a buttress 80 may be molded to include a first leveling pad 81 , and a second leveling pad 82 . The leveling pads 81 and 82 are originally secured to the buttress 80 by a plurality of small runners 83 formed during the molding process. The leveling pads 81 and 82 may be removed from the buttress 80 by breaking the runners 83 . As described in more detail below, the leveling pads 81 and 82 may be positioned under a lower flange 84 of buttress 80 to provide support during assembly of the pool 1 . The buttress 80 may also include a known stake anchoring pin 85 , and may include a third plumbing cradle 86 .
[0041] With reference to FIG. 14 , the first leveling pad 81 includes a first portion 88 having a height H 1 that is about 0.50 inches, and a relatively thin portion 89 having a height H 2 that is about 0.25 inches. Sidewalls 90 and 91 are relatively thin to reduce the amount of material needed to fabricate the leveling pad 81 , and also to provide for quicker cooling, shorter molding cycle times, and reduced distortion during fabrication.
[0042] With further reference to FIG. 15 , the second leveling pad 82 includes a relatively large portion 93 having a height H 3 that is about 0.75 inches, and a relatively thin portion 94 that has a height H 2 of about 0.25 inches. The leveling pad 82 includes sidewall portions 90 and 91 that are relatively thin to facilitate fabrication in substantially the same manner as described above in connection with the leveling pad 81 of FIG. 14 .
[0043] During assembly of the pool 1 , the leveling pads 81 and 82 may be positioned under the lower flange 84 of buttress 80 to provide support. Various spacer heights can be achieved utilizing the leveling pads 81 and 82 as illustrated in FIGS. 16A-16E . With reference to FIG. 16A , a height of 0.25 inches can be achieved utilizing either the first leveling pad 81 or the second leveling pad 82 by positioning the thin portion 89 or 94 having a height H 2 under the lower flange 84 of buttress 80 . As illustrated in FIG. 16B , a spacer height of 0.50 inches can be achieved by positioning the larger portion 88 of leveling pad 81 having a height H 1 (0.50 inches) under the flange 84 of buttress 80 . With reference to FIG. 16C , a height of 0.75 inches can be achieved by positioning the thick portion 93 of the second leveling pad 82 having a height H 3 (0.75 inches) under the flange 84 of buttress 80 . A spacer height of 1.00 inches can be achieved by positioning the thin portion 89 of first leveling pad 81 on the thick portion 93 of leveling pad 82 to thereby provide a height H 4 (1.00 inches) that is equal to H 2 (0.25 inches) plus H 3 (0.75 inches). Finally, a height H 5 of 1.25 inches can be achieved by positioning the large portion 88 having a height of 0.50 inches of first leveling pad 81 on the large portion 93 having a height H 3 (0.75 inches) of the second leveling pad 82 as illustrated in FIG. 16E .
[0044] The leveling pads 81 and 82 thereby provide a very quick and easy way to level the buttress 80 and pool 1 during fabrication. By utilizing the different heights and combinations of leveling pads illustrated above, a wide range of spacer heights can be achieved. It will be readily apparent that additional height combinations may be achieved utilizing additional leveling pads 81 and 82 from additional buttresses 80 . Alternately, additional leveling pads could be separately supplied. Also, it will be readily apparent that the heights of the leveling pads may be different heights than the examples discussed about to provide proper spacing if required.
[0045] With further reference to FIG. 17 , a pair of wedge blocks 97 may also be utilized to provide for spacing below a buttress. Wedge blocks 97 include a flat surface 98 and an angled surface 99 . In use, the angled surfaces 99 contact one another, such that the overall height H provided by the blocks 97 can be adjusted by horizontally shifting of the blocks 97 relative to one another. Also, the edges 99 may include a plurality of steps shown in dashed lines. The steps 96 on blocks 97 engage one another to provide adjustment for the height H without sliding of the blocks 97 relative to one another.
[0046] A pool according to the present invention may be quickly constructed, and also provides a very durable and secure structure. The buttresses, wall components, and peg and wedge connectors are constructed of a durable, non-corrosive material that also provides for a durable structure. The panels may have a wide variety of shapes, such as 90° inside and outside corners of relatively small or relatively large radiuses. Also, the panels may have a 135° configuration to provide for octagons “Lazy Grecians”, “Lazy L's”, or a wide variety of other configurations as required for a particular application. | A wall and buttress construction for swimming pools in which deck support extensions can be secured to the top of the buttresses. The wall includes a plurality of panels having end flanges at the sides of the panels, and a double slotted peg is provided. One of the slots is shorter to receive a wedge when a peg is placed through two abutting panel end flanges, and the other slot being longer to accommodate a wedge when the peg is being used to join a brace as well as two abutting end flanges. The end flanges have elongated openings therethrough for receiving the pegs that are oriented diagonally, rather than either vertically or horizontally. The elongated openings, pegs and wedges are easily visible/accessible for inserting pegs as a result of the diagonal orientation. | 4 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] The present application claims priority benefit under 35 U.S.C. §120 to, and is a continuation of U.S. patent application Ser. No. 11/171,632, filed Jun. 30, 2005 entitled “Cyanotic Infant Sensor,” now U.S. Pat. No. 7,937,128, which claims priority benefit under 35 U.S.C. §119(e) from U.S. Provisional Application No. 60/586,821, filed Jul. 9, 2004, entitled “Cyanotic Infant Sensor.” The present application also incorporates the foregoing disclosures herein by reference.
BACKGROUND OF THE INVENTION
[0002] Cyanosis is a congenital condition in which blood pumped to the body contains less than normal amounts of oxygen, resulting in a blue discoloration of the skin. The most common cyanotic condition is tetralogy of Fallot, which is characterized by an abnormal opening, or ventricular septal defect, that allows blood to pass from the right ventricle to the left ventricle without going through the lungs; a narrowing, or stenosis, proximate the pulmonary valve, which partially blocks the flow of blood from the right side of the heart to the lungs; a right ventricle that is abnormally muscular; and an aorta that lies directly over the ventricular septal defect. Another cyanotic condition is tricuspid atresia, characterized by a lack of a tricuspid valve and resulting in a lack of blood flow from the right atrium to the right ventricle. Yet another cyanotic condition is transposition of the great arteries, i.e. the aorta originates from the right ventricle, and the pulmonary artery originates from the left ventricle. Hence, most of the blood returning to the heart from the body is pumped back out without first going to the lungs, and most of the blood returning from the lungs goes back to the lungs.
[0003] Pulse oximetry is a useful tool for diagnosing and evaluating cyanotic conditions. A pulse oximeter performs a spectral analysis of the pulsatile component of arterial blood so as to measure oxygen saturation, the relative concentration of oxygenated hemoglobin, along with pulse rate. FIG. 1 illustrates a pulse oximetry system 100 having a sensor 110 and a monitor 140 . The sensor 110 has emitters 120 and a detector 130 and is attached to a patient at a selected fleshy tissue site, such as a thumb or toe. The emitters 120 project light through the blood vessels and capillaries of the tissue site. The detector 130 is positioned so as to detect the emitted light as it emerges from the tissue site. A pulse oximetry sensor is described in U.S. Pat. No. 6,088,607 entitled “Low Noise Optical Probe,” which is assigned to Masimo Corporation, Irvine, Calif. and incorporated by reference herein.
[0004] Also shown in FIG. 1 , the monitor 140 has drivers 150 , a controller 160 , a front-end 170 , a signal processor 180 , a display 190 . The drivers 150 alternately activate the emitters 120 as determined by the controller 160 . The front-end 170 conditions and digitizes the resulting current generated by the detector 130 , which is proportional to the intensity of the detected light. The signal processor 180 inputs the conditioned detector signal and determines oxygen saturation, as described below, along with pulse rate. The display 190 provides a numerical readout of a patient's oxygen saturation and pulse rate. A pulse oximetry monitor is described in U.S. Pat. No. 5,482,036 entitled “Signal Processing Apparatus and Method,” which is assigned to Masimo Corporation, Irvine, Calif. and incorporated by reference herein.
SUMMARY OF THE INVENTION
[0005] The Beer-Lambert law provides a simple model that describes a tissue site response to pulse oximetry measurements. The Beer-Lambert law states that the concentration c i of an absorbent in solution can be determined by the intensity of light transmitted through the solution, knowing the mean pathlength, mpl λ , the intensity of the incident light, I 0,λ , and the extinction coefficient, ε i,λ , at a particular wavelength λ. In generalized form, the Beer-Lambert law is expressed as:
[0000]
I
λ
=
I
0
,
λ
-
mpl
λ
·
μ
a
,
λ
(
1
)
μ
a
,
λ
=
∑
i
=
1
n
ɛ
i
,
λ
·
c
i
(
2
)
[0000] where μ a,λ is the bulk absorption coefficient and represents the probability of absorption per unit length. For conventional pulse oximetry, it is assumed that there are only two significant absorbers, oxygenated hemoglobin (HbO 2 ) and reduced hemoglobin (Hb). Thus, two discrete wavelengths are required to solve EQS. 1-2, e.g. red (RD) and infrared (IR).
[0006] FIG. 2 shows a graph 200 depicting the relationship between RD/IR 202 and oxygen saturation (SpO 2 ) 201 , where RD/IR denotes the ratio of the DC normalized, AC detector responses to red and infrared wavelengths, as is well-known in the art and sometimes referred to as the “ratio-of-ratios.” This relationship can be approximated from Beer-Lambert's Law, described above. However, it is most accurately determined by statistical regression of experimental measurements obtained from human volunteers and calibrated measurements of oxygen saturation. The result can be depicted as a curve 210 , with measured values of RD/IR shown on an x-axis 202 and corresponding saturation values shown on a y-axis 201 . In a pulse oximeter device, this empirical relationship can be stored in a read-only memory (ROM) for use as a look-up table so that SpO 2 can be directly read-out from an input RD/IR measurement. For example, an RD/IR value of 1.0 corresponding to a point 212 on the calibration curve 210 indicates a resulting SpO 2 value of approximately 85%.
[0007] Accurate and consistent pulse oximetry measurements on cyanotic infants have been difficult to obtain. An assumption inherent in the calibration curve 210 ( FIG. 2 ) is that the mean pathlength ratio for RD and IR is constant across the patient population. That is:
[0000] mpl RD /mpl IR =C (3)
[0000] However, EQ. 3 may not be valid when cyanotic infants are included in that population. The reason may lie in what has been observed as abnormal tissue tone or lack of firmness associated with cyanotic defects, perhaps due to reduced tissue fiber. Such differences in tissue structure may alter the mean pathlength ratio as compared with normal infants. A cyanotic infant sensor addresses these problems by limiting variations in the RD over IR mean pathlength ratio and/or by providing a mean pathlength ratio measure so as to compensate for such variations. Alone or combined, these sensor apparatus and algorithms increase the accuracy and consistency of pulse oximetry measurements for cyanotic infants.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] FIG. 1 is a block diagram of a prior art pulse oximetry system;
[0009] FIG. 2 is an exemplar graph of a conventional calibration curve;
[0010] FIGS. 3A-B are a perspective and an exploded perspective views, respectively, of a cyanotic infant sensor embodiment;
[0011] FIGS. 4-5 depict cross-sectional views of a tissue site and an attached pulse oximeter sensor, respectively;
[0012] FIG. 6 depicts a cross-sectional view of a tissue site and an attached cyanotic infant sensor;
[0013] FIGS. 7A-B are plan and cross-sectional sensor head views of a conventional pulse oximeter sensor;
[0014] FIGS. 8-9 are plan and cross-sectional sensor head views of cyanotic infant sensor embodiments; and
[0015] FIG. 10 is an exemplar graph of a calibration surface incorporating a mean pathlength ratio measure.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0016] FIGS. 3A-B illustrate one embodiment of a cyanotic infant sensor. The sensor has a light absorbing surface, as described with respect to FIGS. 4-6 , below. The sensor also has a detector window configured to limit the detector field-of-view (FOV), as described with respect to FIGS. 7-9 , below. Advantageously, these features limit mean pathlength ratio variations that are particularly manifest in cyanotic patients.
[0017] The sensor emitters and detector are also matched so as to limit variations in the detector red over IR DC response, i.e. RD DC /IR DC , that are not attributed to variations in the mean pathlength ratio (EQ. 3). Such matching advantageously allows for measurement and calibration of the mean pathlength ratio, as described with respect to FIG. 10 , below. In one embodiment, cyanotic infant sensors 300 are constructed so that:
[0000] λ RD ≈c 1 ; λ IR ≈c 2 (4)
[0000] I 0,RD /I 0,IR ≈c 3 ; for i DC (RD), i DC (IR) (5)
[0000] RD DC /IR DC ≈c 4 (6)
[0000] That is, sensors 300 are constructed from red LEDs and IR LEDs that are each matched as to wavelength (EQ. 4). The LEDs are further matched as to red over IR intensity for given DC drive currents (EQ. 5). In addition, the sensors 300 are constructed from detectors that are matched as to red over IR DC response (EQ. 6).
[0018] As shown in FIG. 3A , the sensor 300 has a body 310 physically connecting and providing electrical communication between a sensor head 320 and a connector 330 . The sensor head 320 houses the emitters and detector and attaches to a patient tissue site. The connector mates with a patient cable so as to electrically communicate with a monitor. In one embodiment, a sensor head surface 324 is constructed of light absorbing material.
[0019] As shown in FIG. 3B , the sensor 300 has a face tape 330 , a flex circuit 340 and a base tape 360 , with the flex circuit 340 disposed between the face tape 330 and the base tape 360 . The flex circuit 340 has a detector 342 , an emitter 344 with at least two light emitting diodes (LEDs), an information element 346 , and contacts 348 disposed on a connector tab 349 . Neonatal sensors having a detector, LEDs, an information element, contacts and connector tab are described in U.S. Pat. No. 6,256,523 entitled “Low-Noise Optical Probes,” which is assigned to Masimo Corporation, Irvine, Calif. and incorporated by reference herein. In one embodiment, the face tape 350 and base tape 360 are constructed of Betham tape having attached polyethylene head tapes 351 , 361 . In a particular embodiment, the base head tape 361 is made of black polyethylene, and the face head tape 351 is made of white polyethylene. In one embodiment, a clear tape layer is disposed on the base head tape 361 tissue side over the detector window 362 . The base head tape 361 has a detector window 362 and an emitter window 364 each allowing light to pass through the base head tape 361 . In one embodiment, the base head tape 361 has a 4 mil thickness and the flex circuit has a 10 mil thickness. The combined 14 mil material thickness functions to limit the detector FOV, as described with respect to FIGS. 6 and 8 , below.
[0020] FIGS. 4-6 illustrate some of the pathlength control aspects of a cyanotic infant sensor 300 . FIG. 4 depicts a fleshy tissue site 10 for sensor attachment, such as a finger or thumb 400 . The tissue 10 has an epidermis 12 , a dermis 14 , subcutaneous and other soft tissue 16 and bone 18 .
[0021] FIG. 5 depicts a conventional pulse oximetry sensor 20 having a detector 22 , an emitter 24 and a tape 26 attached to the fleshy tissue 10 . Transmitted light 30 propagating from the emitter 24 to the detector 22 that results in a significant contribution to pulse oximetry measurements passes through and is absorbed by the pulsatile blood in the dermis 14 . A portion of the transmitted light 30 is scattered out of the epidermis 12 and reflected by the tape 26 back into the fleshy tissue 10 . The detector field-of-view (FOV) 40 is relatively wide and, as a result, the detector responds to transmitted light 30 that has propagated, at least in part, outside of the fleshy tissue 10 .
[0022] FIG. 6 depicts a cyanotic infant sensor 300 that is configured to limit variations in the mean pathlength ratio. In particular, the sensor 300 has a light absorbing tape inner surface 324 that reduces transmitted light reflection back into the tissue site 10 , as described with respect to FIGS. 3A-B , above. Further, the detector 342 has a limited FOV 50 so as to reduce the detection of transmitted light that has propagated outside of the tissue site 10 , as described in detail with respect to FIGS. 7-9 , below.
[0023] FIGS. 8-9 illustrate cyanotic infant sensor embodiments having a limited detector field-of-view (FOV). FIGS. 7A-B illustrate a conventional sensor 700 having a tape portion 760 , a detector window 762 and a detector 742 having a relatively wide FOV 701 . In particular, the window thickness does little to restrict the FOV. FIGS. 8A-B illustrate one embodiment of a cyanotic infant sensor 300 having a material portion 360 , a detector window 362 and a detector 342 having a restricted FOV 801 . In particular, the material thickness 360 functions to define the FOV 801 . In one embodiment, the material thickness 360 comprises a flex circuit thickness and a base head tape thickness, as described with respect to FIG. 3B , above. FIGS. 9A-B illustrate another embodiment of a cyanotic infant sensor 900 having a material portion 960 , a detector window 962 and a detector 942 having a restricted FOV 901 . In particular, an O-ring 980 deposed around the window 962 defines the FOV 901 .
[0024] FIG. 10 depicts an exemplar calibration surface 1000 for a cyanotic infant sensor 300 ( FIGS. 3A-B ) calculated along a DC response ratio axis 1001 , a ratio-of-ratios axis 1003 and a resulting oxygen saturation axis 1005 . Matching the emitters and detectors, as described with respect to FIG. 3A , above, allows for pathlength calibration. In particular, variations in the detector DC response ratio (RD dc /IR dc ) are attributed to variations in the mean pathlength ratio (EQ. 3). As such, a calibration surface is determined by statistical regression of experimental measurements obtained from human volunteers and calibrated measurements of oxygen saturation, as is done for a conventional calibration curve ( FIG. 2 ). A calculated DC response ratio 1001 in combination with a conventionally calculated ratio-of-ratios 1003 is then used to derive an oxygen saturation 1005 for the calibration surface 1000 .
[0025] A cyanotic infant sensor has been disclosed in detail in connection with various embodiments. These embodiments are disclosed by way of examples only and are not to limit the scope of the claims that follow. One of ordinary skill in art will appreciate many variations and modifications. | A pulse oximetry sensor comprises emitters configured to transmit light having a plurality of wavelengths into a fleshy medium. A detector is responsive to the emitted light after absorption by constituents of pulsatile blood flowing within the medium so as to generate intensity signals. A sensor head has a light absorbing surface adapted to be disposed proximate the medium. The emitters and the detector are disposed proximate the sensor head. A detector window is defined by the sensor head and configured so as to limit the field-of-view of the detector. | 0 |
FIELD OF THE INVENTION
This invention relates to multiple sensor communication and, more particularly, to apparatus and methods for achieving multi-channel communication with many sensor devices connected across a two-wire communication path in a seismic streamer cable.
BACKGROUND OF THE INVENTION
In a marine seismic survey, a surveying vessel tows one or more seismic cables or streamers. Each streamer is outfitted with distributed seismic transducers, namely hydrophones, and position-control devices and position-determining sensors, such as cable-leveling birds, compasses, depth (pressure) sensors, and hydroacoustic ranging transceivers. Data from the hydrophones are sent to a controller on board the vessel via a high-speed data link, which could be an optical-fiber link. Data from the position sensors, on the other hand, are typically transmitted to the controller via a two-wire, twisted-pair line, each wire of the pair being no larger than size 22 AWG. Sensors are connected along the twisted pair in one of two ways. First, in-streamer sensors are connected in parallel directly across the twisted pair. Typically, in-streamer sensors are also powered over the twisted pair. Second, outlying sensors, such as those sensors residing in cable-leveling birds or hydroacoustic transceivers, are individually coupled to the twisted pair by means of a coupling coil connected in parallel across the twisted pair. Each outlying sensor has an individual, associated coil in the streamer.
The coupling coils in the streamer are conventionally tuned to the same frequency and typically have a fairly high selectivity, or Q, giving the two-wire communication system a narrow bandwidth and a relatively low data rate. The high Q further makes tuning of the transmitting frequency critical for effective communication. Because noise generated in the neighboring power system for the high-speed hydrophone data link occurs at a dominant frequency of about 2 kHz with harmonic level decreasing with frequency to beyond 100 kHz, typical two-wire communication takes place at about 25 kHz. Conventional communication is achieved my means of frequency-shift-keying (FSK) modulation. Other variations of angle modulation, such as quadrature-phase-shift keying (QPSK) and bipolar-phase-shift keying (BPSK), are also commonly used. Carrier frequencies on the order of 20 kHz-30 kHz are common. Proper tuning of the carrier frequency is critical to achieve a signal-to-noise ratio adequate for effective communication. Thus, present-day two-wire streamer communication relies heavily on a properly tuned system.
Prior art two-wire communication with position sensors on streamers has generally been realized by half-duplex, single-channel communication schemes. Consequently, only one sensor is allowed to send data at a time. Likewise, no sensor may send data while the controller is communicating. Such limitations have only recently become important. Several developments promise to make the half-duplex, single-channel communication system inadequate to meet expected demands in position-determining requirements. First, hydroacoustic ranging systems are seeing more widespread use. The positioning accuracy they provide, particularly in multi-streamer applications, is necessary to support the increased accuracy being demanded of seismic surveys. Each hydroacoustic transceiver typically transmits much more data to the controller than other sensors, such as compasses and depth sensors. Second, maximum streamer lengths of 10 km are expected to become commonplace, in contrast to 6 km today. Longer streamers accommodate more sensors on a single twisted pair with the concomitant increase in data traffic. Third, in the continuing quest for greater accuracy, today's typical spacings of every 300 m for depth sensors and compasses may well be replaced by spacings of 100 m, for a threefold increase in the number of these sensing devices. Fourth, to avoid interference with seismic measurement activity, availability of the communication system for data traffic may be limited to two seconds or less every seismic shot interval, which is typically ten seconds. Thus, in view of the expected expanded use of acoustics, longer streamers, closer sensor spacing, and narrower data transmission intervals, prior art two-wire streamer communication systems will be inadequate to handle the increased data traffic.
Aside from being unable to handle the increased data traffic, prior art two-wire communication systems do not predict communication failures. Failure to terminate the twisted-pair line properly causes standing waves on the line that can null out the signals at sensor positions along the line. Broken or shorted connections are another source of faulty communications. Finally, saltwater leakage causes deterioration of the communication link over time. Prior art communication systems do not recognize deterioration of the communication link until it is all but dead.
Therefore, one object of the invention is reliable, high throughput data communication over existing twisted-pair lines with many sensors distributed along marine seismic streamers up to 10 km long. It is a further object of the invention to permit early diagnosis of deteriorating communication so that prompt corrective action can be taken.
BRIEF DESCRIPTION OF THE DRAWINGS
For a further understanding of the nature and objects of the present invention, reference should be made to the following detailed description, including the accompanying drawings, in which:
FIG. 1 is side view of a seismic surveying vessel towing a streamer outfitted with sensing and streamer control devices in communication with a controller aboard the vessel in accordance with the invention;
FIG. 2 is a partial cutaway schematic view of a section of a conventional seismic streamer representing two twisted-pair communication lines, one showing parallel-connected coupling coils, in-line devices, and a line termination;
FIG. 3A is a family of curves representing the signal strength as a function of frequency for various distances from a 20 dBV (10 V) signal source for a conventional 22 AWG twisted-pair communication line with a number of low Q coupling coils distributed therealong;
FIG. 3B is a family of curves as in FIG. 3A, but for a higher Q coupling coil, along with the interference spectrum in the streamer environment;
FIG. 4A is a family of curves representing the group of delay as a function of frequency for various distances from a signal source, corresponding to the line with low Q coupling coils having the signal strength characteristic of FIG. 3A;
FIG. 4B is a family of curves as in FIG. 4A, but corresponding to the high Q coupling coil having the signal strength characteristic of FIG. 3B;
FIG. 5 is a partial schematic block diagram of a preferred embodiment of the communication apparatus of the invention;
FIG. 6 is a schematic block diagram of another embodiment of the invention showing some components in more detail than in FIG. 5;
FIG. 7 is a schematic diagram of a multiplexer circuit used in the invention to monitor electrical transmission and reception parameters;
FIG. 8 is a timing diagram depicting an exemplary polling and response sequence according to the invention; and
FIG. 9 is a chart showing the preferred channel assignment of the communication system of the invention.
SUMMARY OF THE INVENTION
These and other objects are achieved by the present invention, which provides a multi-channel, two-wire communication system for sending commands and data requests to and receiving data rom many positioning sensors and cable-leveling devices distributed along a seismic streamer. The apparatus of the invention includes a central controller comprising an intelligent modem that can scan the many streamer devices for cable-positioning data each seismic shot interval. By referring to an equipment table stored in memory, the intelligent modem polls each device in an efficient and orderly fashion by transmitting message signals over an outbound channel. Responses from the polled devices in the form of message signals are received by the modem over one or more inbound channels different from the outbound channel. According to a preferred embodiment, a modem has the capability of transmitting outbound commands or data request messages one of four channels as frequency-modulated signals and of receiving frequency-modulated response messages on one of thirteen inbound channels.
My measurements and modeling of the loss and group delay characteristics of conventional 22 AWG and smaller twisted-pair, coupling-coil-laden streamer communication lines revealed relatively flat loss and group delay characteristics above conventional coil resonant frequencies of 20 kHz-25 kHz up to about 100 kHz. My further measurements of the power system interference spectrum level revealed signal-to-noise ratios adequate for successful communication at frequencies from about 200 kHz up to 100 kHz. The novel streamer communication system of the invention takes advantage of the newly recognized loss and group delay characteristics and the interference spectrum by operating over a multitude of channels between about 20 kHz and 100 kHz, instead of a single channel as is conventionally done, thereby permitting the much higher data throughput rates necessary for advanced cable-positioning solutions. The invention additionally provides an operator on board the survey vessel with communication quality and performance measures, such as inbound and outbound signal strengths and signal-to-noise ratios, ac line impedance, dc line load, false carrier detections, and message errors for detection of streamer problems earlier than heretofore possible.
DETAILED DESCRIPTION OF THE INVENTION
A seismic surveying vessel 20 is depicted in FIG. 1 towing a seismic streamer 22 beneath the sea surface 21. Distributed along the length of the streamer 22 are in-streamer sensors 24A-D, such as compasses and depth sensors, and outboard devices, such as cable-leveling birds 26A-B and acoustic ranging transceivers 28A-B. For brevity, all such devices are hereinafter referred to generally as sensors. The outboard sensors are connected to the streamer 22 by means of collars 27 clamped around the streamer. The streamer includes a front-end marker buoy 30 tethered to the streamer 22 by a tether cable 32 and a tail-end buoy 34 tethered to the end of the streamer 22 by a tether cable 36. The sensors 24, 26, and 28 are all in communication with a central controller 38 on board the vessel 20. Hydrophones (not shown) are also distributed along the streamer 22 for detecting seismic energy generated by a seismic source (also not shown) and reflected off geologic structures in the earth's surface. The birds 26A-B, such as the Model 5000 manufactured by DigiCOURSE, Inc., the subsidiary of the assignee of this invention, are used to control the depth of the streamer 22. Outfitted with heading sensors and depth sensors, a bird 26 can also communicate heading and depth data to the on-board controller 38 for use in predicting the shape of the streamer 22. The acoustic ranging transceivers 28A-B transmit transit time information to the controller 38 also for use in estimating the shape of the streamer 22. Of course, a typical deployment would include many more of such sensors and more streamers than shown in FIG. 1.
Communication between the sensors and the on-board controller is effected over one or more two-wire lines running through the streamer as shown in FIG. 2. The cutaway side view of a portion of a streamer 40 reveals, in this example, two twisted-pair lines 42A-B. An outboard bird 44, clamped to the streamer 40 by a collar (not shown), communicates with the on-board controller by means of inductive coupling between an in-streamer primary coil 46A and a secondary coil 48A within the bird 44 or its collar. A capacitor 45A, in series with the primary coil 46A, blocks direct current used to power in-streamer sensors. Control signals are received by the bird electronics 50 to control the wings of the bird and, thereby, the depth of the streamer. The bird electronics also measure various operating parameters, such as depth, heading, wing angle, temperature, and battery status, and send such data to the controller upon request. In a similar manner, the controller communicates over the same line 42A with an acoustic ranging transceiver 52 and its internal electronics package 54 by means of a similar primary coil 46B and capacitor 45B and secondary coil 48B. As can be seen, each outboard device is put into communication with the line 42A by means of a corresponding coil 46 connected in parallel across the twisted-pair line. In-streamer devices, such as a heading sensor 56, are connected directly in parallel across the lines of the line 42B. To prevent line reflections that can cause nulls in the communication signals, the line 42B is terminated with its characteristic impedance 58. Thus, a twisted-pair line over which cable-position sensors communicate with the on-board controller contains a number of coupling coils or in-streamer devices all connected in parallel across the line. Each sensor has a unique address or serial number identifier for communication addressing. An individual 10 km twisted-pair line could include up to 377 parallel sensors. For long streamers having more sensors than a single twisted-pair line can handle, additional lines could be used as exemplified by the two twisted-pairs 42A and 42B in FIG. 2.
In a conventional twisted-pair communication system, with a wire size of 22 AWG and having a number of identical low Q coupling coils distributed therealong, the signal strength characteristic is typified by FIG. 3A. For convenience of comparison with the interference spectrum, the signal strength of a signal 10 transmitted at a level of 20 dBV, or 10 V, by a signal source is plotted as a function of frequency for various distances from the source, instead of the reciprocal loss characteristic. The signal strength characteristic for a line having a number of high Q coils is shown in FIG. 3B. For example, in FIG. 3A, at 50 kHz with low Q coils, the signal strength (-50 dB) at a distance of 8 km from the signal source is about 19 dB less than the signal strength (-31 dB) at a distance of 4 km. It is important to notice that, although the signal strength decreases with frequency, so does the interference spectrum level 60, which decreases with frequency from 20 kHz to 100 kHz, as shown in FIG. 3B. Furthermore, the group delay characteristic between 20 kHz and 100 kHz for both high and low Q coils, shown in FIGS. 4A and 4B, is relatively flat. A non-flat group delay characteristic for which the delays of the upper and lower frequencies of a frequency-modulated signal differ by more than about 0.1 ms at 2400 baud degrades the performance of conventional modems. Thus, a significant bandwidth is available for frequency-modulated communication over existing twisted-pair lines above the coil resonant frequency of about 20 kHz.
Instead of limiting communication to the relatively narrow bandwidth of the coil resonance characteristic, the present invention takes advantage of the wide bandwidth available above 20 kHz to communicate efficiently with many sensors. The preferred communication scheme is a multi-channel approach, in which 17 individual narrow-band channels from about 20 kHz to 100 kHz are used to permit full-duplex communication with many sensors distributed along a streamer. Channels are limited to below 100 kHz, because, at higher frequencies, the two-wire line behaves more like a distributed parameter transmission line than a lumped parameter circuit. Such a multi-channel approach permits sensors operating on separate channels to communicate simultaneously. Because of the signal strength characteristics and interference spectrum shown in FIG. 3, channels are assigned to sensors according their distances from the on-board controller for best signal-to-interference ratios. Lower frequency channels are assigned to those sensors farthest from the controller. One skilled in the art will recognize that the invention could likewise be used with communication lines other than twisted-pair lines, as long as they exhibit similar signal strength and group delay characteristics.
A block diagram of the multi-channel communication system of the preferred embodiment of the invention is shown in FIG. 5. Communication with streamer sensors is realized by a modem configured around a modem processor 70 having a RAM scratchpad memory 74 and non-volatile memory 72, such as ROM, for program storage. The modem processor sends and receives sensor commands and data from the other processing equipment on board the survey vessel over a parallel system bus 76, such as a VME bus. Bus control circuits 78 interface the modem processor 70 with a communication processor 80 in communication with other on-board processing equipment. (The central controller 38 in FIG. 1 includes the modem processor 70 and the communication processor 80.) Preferably, data are passed between the communication processor 80 and the modem processor 70 through designated memory areas in a dual-ported RAM 82 shared by the two processors. Interrupts from the communication processor 80 signifying the start of a sensor scan cycle are also passed to the modem processor 70 over the system bus 76.
The modem processor 70 communicates with the individual sensors over twisted-pair lines 84A-H each containing a number of parallel-connected coils or in-streamer sensors. For simplicity each twisted-pair line is represented by a single line in FIG. 5. Each line is connected to an individual modem physical layer 86A-H. A typical physical layer comprises a transmit path, a receive path, and an isolation transformer 88.
The transmit path includes a digital transmitter 90 controlled by the modem processor 70. The digital transmitter 90 is programmed or preset to synthesize a frequency-modulated digital signal at its output, the modulation being a function of the data to be transmitted. The digital signal is applied to a D/A converter 92 to produce an analog frequency-modulated signal, which is filtered by a bandpass filter 94 to remove digital noise and out-of-channel signal, and amplified by a power amplifier 96 before being coupled onto the line 84A via the transformer 88 for transmission to the sensors. Data transmitted by a sensor are coupled into the physical layer 86A through the transformer 88. A bandpass filter 98 eliminates low-frequency interference, such as seismic interference and power system interference, and transmitter interference from the receiver. The filtered signal is buffered in a pre-amp 100 before being applied to an A/D converter 102, which converts the analog receive signal into a digital signal to be demodulated by a digital receiver 104. The demodulated data are then sent to the modem processor 70 from the physical layers 86A-H over UART ports 106A-H. Although only two lines 108A-H and 109A- H are shown for each UART port 106A-H, a full RS-232C handshaking link is implemented, as will be described hereinafter. Although the block diagram of FIG. 5 shows eight physical layers, it should be recognized that realizations having more physical layers are within the scope of the invention.
In a preferred embodiment, the transmitter 90 and the receiver 104 are realized by a multiplicity of digital-signal-processing (DSP) integrated circuits, such as the Model TMS320C40 manufactured by Texas Instruments, Inc., Dallas, Tx. Such a device allows great flexibility in selecting carrier frequencies and modulation schemes. In this embodiment, however, a minimum frequency-shift-keying modulation (MSK) scheme is used whereby a logic low data bit causes a frequency of f c -600 Hz to be transmitted and a logic high data bit causes a frequency of f c +600 Hz to be transmitted where f c is the transmit channel center frequency. Data bit rates of 2400 baud make the system compatible with the group delay characteristic of the channel. As a transceiver, the DSP integrated circuit is capable of full duplex operation, i.e., simultaneous transmission and reception, as well as simultaneous multi-channel reception.
In another embodiment, shown in the schematic block diagram of FIG. 6, the transmit and receive functions of the physical layer are performed by analog and digital circuitry not including a DSP integrated circuit. Each transmitter 111A-B includes a digital phase accumulator 110 whose output is a digital count incremented at a rate determined by the transmit clock signal 112, the transmit channel frequency setting 114, and the data bit 116 to be transmitted. The transmit clock signal may be derived from a bus clock signal 118 by a frequency divider 120. For a given transmit clock rate and a selected transmit channel, the rate of the digital count out of the phase accumulator is determined by the transmit data. Preferably, the transmit data 116 are sent serially to the phase accumulator 110 from a TX line of a UART on the modem processor using standard NRZ asynchronous serial communication, including start and stop bits. The sequence of data logic levels, alternating between highs and lows, adjusts the output count between two rates, which are converted into two respective frequencies by sine ROM 122 and D/A converter 124, thereby producing an MSK-modulated signal at the output of the D/A converter 124. The phase accumulator and sine ROM functions can be implemented by a single integrated circuit, such as an HSP45102 numerically controlled oscillator, manufactured by the Harris Corporation, Melbourne, Fla. For a logic low data bit, the frequency is selected to be f c -600 Hz; for a logic high data bit, the frequency is selected to be f c +600 Hz, where f c is the transmit channel center frequency. The start of the conversion process in the D/A converter 124 is controlled by the transmit clock input signal 112, which is the clocking rate of the digital signal. The modem processor can also control the amplitude of the output of the D/A converter and, hence, the transmitted energy, by means of a level adjust signal 128. The analog signal out of the A/D converter 124 is filtered by an adjustable bandpass filter 130, which removes digital quantization noise and out-of-channel signals. The filtered analog signal is amplified in a power amplifier 132 terminated in adjustable line-matching impedance 134 for maximum power transfer to the communication line. Other similar transmitters, operating on different channels, may be interconnected into the communication system, as indicated by a transmit signal summer 126. Voltage and current monitoring circuits 135 and 137 measure the output ac voltage and current levels at the modem side of an isolation transformer 136. Peak-hold detector circuitry reset by a processor-controlled signal (PK DET RESET) 133 is used to measure the voltage across and the current through the transformer 136 to be read by the modem processor. Power to drive in-streamer devices over the communication line 138 is provided by a dc power supply 140, whose output voltage and current can be monitored by the modem processor 70 through isolated voltage and current monitoring circuits 139 and 141, comprising filtered buffers and isolation amplifiers to isolate the line electrically from the modem processor 70. The dc power is coupled into the line 138 as indicated by a signal summer 142. Of course, the transmit signals could alternatively be summed on the line side of the transformer 136 by a network such as the signal summer 142, instead of by the transmit signal summer 126. Thus, the transmitter converts a serial asynchronous NRZ data stream from a UART controlled by the modem processor into an MSK-modulated signal at the same data rate as the serial UART data. The MSK-modulated transmit signal is summed with dc power for in-streamer devices and sent down the communication line for decoding by the appropriately addressed sensors. In a full-duplex system, responses from various sensors may occur simultaneously on different channels. Simultaneous receive channels are implemented in the embodiment of FIG. 6 by additional receivers for each receive channel. A description of the operation of one receiver suffices to describe the operation of all, which are identical, except for being tuned to receive on separate channels. Four receivers 144A-D are shown in FIG. 6. The input to each receiver is taken from the transformer 136. Although the receivers are shown connected to the modem side of the transformer 136 in FIG. 6, they could alternatively be coupled through individual transformers connected to the line side of the transformer 136. Each receiver, as exemplified by receiver 144A, includes an adjustable notch filter 146 for attenuating the transmit frequency coupled into the receiver. The filtered signals from the streamer sensors are buffered in a pre-amp 148 and further filtered in an adjustable bandpass filter 150 tuned to the designated receive channel frequency. The filtered signal is then limited in a limiter 152 to preserve phase information representing the data and demodulated in an FM demodulator 154. In the embodiment described by reference to FIG. 6, the signals from the sensors to the modem are MSK-modulated signals similar to the signals transmitted to the sensors as previously described. In fact, in the preferred embodiment, each sensor has one transmit path and one receive path similar to those on the modem. The demodulator 154 is tuned to the designated receive channel by means of a receive clock signal 156 and a signal representing the receive channel setting 158. The receive clock signal 156 may be derived from a bus clock signal 118 by a frequency divider 160. The demodulator 154 can be realized by an integrated circuit, such as the 74HC297 digital phase-locked-loop manufactured by Texas Instruments. The demodulator 154 indicates to the modem processor that the carrier has been detected via a CARRIER DETECT signal 162. The demodulated receive data 164 is sent to an RX line on a modem processor UART in the conventional NRZ asynchronous format for handling by the message translation logic.
To measure the power level (SIGNAL STRENGTH) of the received signal from a given sensor, the output of the bandpass filter 150 is detected by signal strength monitoring circuitry 151, including, for example, a logarithmic amplifier for dynamic range and a peak-hold detector. As realized by the logic circuit including inverter 153 and OR gate 155, the peak-hold detector can be reset either by the processor-controlled signal PK DET RESET 133 or by the CARRIER DETECT signal 162 whenever the FM demodulator 154 detects no carrier.
Although there are many ways to read and control the operation of the modem transmitters and receivers, the preferred method is to use asynchronous NRZ communication between a UART on the modem processor and the transmitter and receiver circuits. The full RS-232C handshaking protocol is used with, for example, CARRIER DETECT being read by DCD (data carrier detect) and transmitter D/A conversion being enabled by RTS (request to send).
In addition to its ability to send and receive MSK-modulated messages over streamer communication lines, the system of the invention can monitor communication performance. As described with reference to FIG. 6, the transmitted voltage and current for each transmitter channel, the dc voltage and current, and the received signal strength for each receiver channel are measured by conventional circuitry including, for example, operational amplifier circuits.
The multiplexer circuit of FIG. 7 is used to select the various measured quantities for reading by the modem processor. Once again, just as for the transmitters and receivers, communication between the modem processor and the multiplexer circuit is via asynchronous NRZ communication. The TX and RX lines of a modem processor UART are connected to the DATA IN and DATA OUT lines of UART chip 170. The modem processor selects a parameter to be read by transmitting to the UART 170 a byte containing a board address, a parameter address, and a read bit. The serial byte received by the UART is presented in parallel to a latch 172, which selects one of 32 analog measurement channels 175 in multiplexers 174, as long as the board is also selected. Up to four boards can be addressed, permitting a total of 128 measurable quantities, including the ac voltage and current V ac and I ac , the dc voltage and current V dc and I dc , and the signal strengths of each receiver (SIGNAL STRENGTH). The board address is set by a pair of address switches 176 in conjunction with a digital comparator 178. Further address decoding is performed by logic gates 180 and 182. If the board is addressed, one of the analog measurement signals is directed to an A/D converter 184 through one of the multiplexers 174. A read command sent from the modem UART and processed through a logic gate 186 triggers one-shot 188 to generate a convert pulse to start the conversion process in the A/D converter 184. Upon completion of the conversion of the selected measured quantity, the converter 184 generates a conversion complete signal that triggers another channel of the one-shot 188, which generates a pulse to output the converted data from the converter 184 through the UART 170 serially to the modem processor UART over the DATA OUT line. In this way, the many measurable quantities can be easily read.
The measurable quantities are important in diagnosing problems in the communication system. With the test lines shown in FIG. 6, the system can measure and store the following quantities:
1. transmit voltage and current on each transmit channel;
2. background noise on the transmit channel by measuring the transmit voltage and current while not transmitting;
3. received signal strength for each responding sensor;
4. receiver background noise by measuring the signal strength on the receive channel while no data are incoming on that channel; and
5. dc voltage and current supplied to in-streamer devices.
From the first four quantities in the list, the transmit and receive signal-to-noise ratios can be computed by the modem processor 70. Any significant decrease in these signal-to-noise ratios may indicate problems or defects in the streamer, such as salt-water leakage. Likewise, any significant change in the dc voltage and current can indicate short or open circuits along the streamer. Furthermore, sensors capable of measuring the strength of the signals they receive can pass such data to the modem processor for further detailed analysis. With this capability, for example, the signal strength or signal-to-noise ratio as a function of position along the streamer can be determined and displayed to an operator, who can watch for signs of signal degradation, which could indicate problems such as broken or shorted wires in the streamer, an improperly matched termination, and salt-water leakage.
To supplement the signal measurements, communication performance statistics are also computed by the modem processor 70 for each sensor. For example, if a sensor does not respond to a poll request for data, the modem processor 70 increments the number of incomplete polls for that sensor. If the response from a sensor is received with checksum errors, indicating a transmission error, the modem processor 70 increments the bit error counter for that sensor. If the carrier frequency is detected by the receiver when no response is expected, the modem processor 70 increments the number of false carrier detections on that channel. All of the communication performance data are stored in the dual-port RAM 82 for access by the communication processor 80.
As previously described, the preferred embodiment of the invention provides for seventeen channels between about 20 kHz and 100 kHz for communication with sensors over a twisted-pair line. Four of the channels are reserved as outbound, or transmit, channels; thirteen of the channels are inbound, or receive, channels. Preferably, the channel center frequencies are sequentially spaced every 4800 Hz from about 20 kHz to about 100 kHz. Such a spacing is sufficient to provide 85 dB of adjacent channel interference rejection for the 600 Hz-deviated, MSK-modulated signals of the invention. Analysis of the lengths of the required polling (outbound) messages and the response (inbound) messages at a conventional transmission rate of 2400 baud suggests the assignment of channels shown in FIG. 9 to optimize throughput and number of sensors.
In other words, for transmit channels 1, 6, and 11, up to four receive channels can be associated. For transmit channel 16, one receive channel is associated. In assigning channels to devices on a line, transmit channel 1 is first assigned. Then, inbound receive channel 2 is assigned to the 29 sensors farthest from the modem. The next 29 sensors are assigned to transmit data on inbound receive channel 3. This assignment is repeated from the tail end of the streamer toward the head end until up to 116 sensors are assigned to transmit on receive channels 2-5 and to receive outbound poll requests on channel 1. Once these lower-frequency channel assignments are filled, the process is repeated for channels 6-10, then channels 11-15, and finally, if necessary, channels 16 and 17. In this way, the communication system can support up to 377 sensors on a single twisted-pair line, with the lower frequencies assigned to those sensors farthest from the modem. This optimum arrangement of transmit and receive channels is based on the following assumptions:
1. a complete scan (outbound poll and inbound response) of all sensors on the streamer within one second;
2. an average response message of 8 bytes per sensor;
3. a message data rate of 2400 baud;
4. full-duplex asynchronous serial communication;
5. a poll message of two bytes per sensor; and
6. streamers of up to 10 km in length.
All these assumptions are reasonable in view of imminent surveying demands for greater accuracy in 3-D seismic exploration.
A typical scan sequence over channels 1-5 is depicted in FIG. 8, in which the blocks depict message blocks to and from individual streamer sensors designated by a unique letter. Outbound poll messages from the modem board are transmitted on channel 1 to all sensors that can respond on channels 2-5. As soon as sensor A is polled, it responds on channel 2. Furthermore, as soon as the poll of A is completed, sensor B is polled, and so on until a sensor assigned to each inbound channel is polled. In the meantime, response messages are sent from the sensors over their assigned response channels to the modem. As soon as an inbound message is received on a channel, the next sensor on that channel is polled. As shown in the example of FIG. 8, after sensor D is polled all four inbound channels are busy. As soon as the message from sensor A is completed, channel 2 is available, so that the modem can poll sensor E. By the time the poll of E is complete, the response from sensor C on channel 4 is completed, so that sensor F, which responds on channel 4 can be polled. A sensor having a long message length, such as sensor B on channel 3, is skipped until its inbound channel is clear. Using this poll and response scheme, higher throughput communication is possible.
Any sensors that do not respond or whose messages are erroneous may be repolled at the end of the complete scan. The number of repolls can be set for all devices. Thus, the high throughput allows time for repolling, which can be of significant value in a noisy environment.
The invention as described provides a multi-channel communication system operable on conventional two-wire, twisted-pair lines and capable of handling the high data traffic required to support the positioning accuracies and longer streamers being used in three-dimensional seismic surveying. Although the invention is described with respect to a preferred embodiment, modifications thereto will be apparent to those skilled in the art. Accordingly, those novel features defining the spirit and nature of the invention are set forth with particularity in the following claims. | For use with marine seismic streamers, a two-wire, multi-channel communication system capable of handling the high throughput necessary for effective communication between a central controller aboard a tow vessel and the many sensors deployed along the streamer. The central controller includes an intelligent modem with the capability of transmitting and receiving frequency-modulated message signals on one or more signal lines, such as conventional twisted-pair wires, over a number of individual inbound and outbound frequency channels. In the preferred embodiment, seventeen channels are spread over a frequency band ranging from about 20 kHz to 100 kHz, thereby making available for communication a bandwidth much wider than available in conventional single-channel streamer communication. In this way, many positioning sensors, such as compasses, depth sensors, cable-leveling birds, and acoustic-ranging transceivers, attached to the streamer and each having a transmitter and receiver tuned to one of the modem's inbound and outbound channels, respectively, can be put in communication with the modem. To take advantage of its high throughput capability, the intelligent modem refers to a stored table of individual sensor parameters, such as sensor type, transmit channel, and receive channel, to schedule an efficient scan of the sensors. As a diagnostic tool, the communication system also monitors the quality and performance of the communication link by measuring and recording such parameters as the transmitted and received signal strengths, signal-to-noise ratios, and number of incorrectly received messages. | 6 |
FIELD OF THE INVENTION
[0001] The present invention relates to weakly basic hindered amine compounds having carbonate skeletons.
BACKGROUND ART
[0002] Hindered amine compounds are known to suppress the photodegradation of organic substances such as synthetic resins, and since the stabilization effect is different depending on the structure of the amine and the environment in which it is used, amines with active hydrogen atoms, amines without active hydrogen atoms and alkyloxyamines which are even more weakly basic than tertiary amines, have been considered for this purpose. The idea of introducing a triazine skeleton in order to enhance compatibility with the synthetic resin to be stabilized or its extraction resistance, has also been considered.
[0003] For example, prior art hindered amine compounds, when used with polyolefin resins, had low compatibility with the resin, and since they vaporized from the resin, they had the problem that their stabilization effect did not endure. Moreover, in applications where they came in contact with acid rain and agricultural chemicals, there was also the problem that they were extracted by the acid.
[0004] Hindered amine compounds having a carbonate structure have been proposed in Tokkai-Sho 62-273239 (claims and compounds No. 30, No. 31), Tokkai-Sho 63-75019 (claims and compounds I-19, I-20, I-21), for the purpose of stabilizing polyolefin resins or as a catalyst quencher in the manufacture of oxymethylene (co)polymers.
[0005] However, there is neither any disclosure nor suggestion of weakly basic hindered amine compounds having an alkyloxyamine structure.
[0006] As an example of a weakly basic hindered amine compound, a compound having such an alkyloxyamine structure is proposed in Tokko-Sho 49-40557 (claims), and weakly basic hindered amine compounds having various skeletons are proposed in Tokkai-Hei 1-113368 (claims), e.g., hindered amines having a carboxylate structure, amide structure, carbamate structure or acetal structure.
[0007] Since weakly basic hindered amine compounds show superior resistance to acid extraction, their practical use in polyolefin agricultural films has been proposed, e.g., in Tokkai-Hei 2001-139821 (claims).
[0008] However, there is neither any disclosure nor suggestion of weakly basic hindered amine compounds having a carbonate structure.
[0009] Many hindered amine compounds have been proposed in the prior art, but for example in the case of agricultural films, since light transmissivity (which depends on the stability of the resin in the film) has a major impact on the growth of crops, a hindered amine compound which had a better longer-term stabilization effect was desired.
SUMMARY OF THE INVENTION
[0010] The present invention therefore proposes a hindered amine compound which confers long-term stabilization on synthetic resins, and which shows superior resistance to extraction by acid rain or chemicals.
[0011] The Inventors, as a result of extensive research carried out to resolve this problem, found that the hindered amine compound having a carbonate structure represented with by the general formula (I) or (II) gave excellent long-term stabilization of a synthetic resin, and thereby arrived at the present invention.
[0012] The first invention therefore provides a hindered amine compound represented by the general formula (I) or (II):
[0000]
[0000] (in the formula, R is an alkyl group or a hydroxyalkyl group having 1-30 carbon atoms, or an alkenyl group having 2-30 carbon atoms, and n is an integer from 1-6. When n=1, R 1 is an alkyl group having 1-22 carbon atoms, an alkenyl group having 2-22 carbon atoms, or the group represented by the following general formula (III):
[0000]
[0000] (R is the same alkyl group or hydroxyalkyl group having 1-30 carbon atoms, or alkenyl group having 2-30 carbon atoms as R above).
[0013] When n=2-6, R 1 is an organic group having 2-20 carbon atoms of valency n).
[0000]
[0000] (in the formula, R is an alkyl group having 1-30 carbon atoms or an alkenyl group having 2-30 carbon atoms, R 2 is a hydrogen atom, an alkyl group having 1-22 carbon atoms or an alkenyl group having 2-22 carbon atoms, and A is a single bond, a linear- or branched-alkylene group having 1-12 carbon atoms or an alkylene group having ether linkage; n is an integer from 2-6; X is —C(═0)-, a linear- or branched-alkylene group having 4-40 carbon atoms with a terminal —C(═O)O—, a linear- or branched-alkylene group having 4-40 carbon atoms with a carbonic acid ester linkage, or an organic group having 6-30 carbon atoms with 3-6 terminal —O—C(═O)—).
[0014] The second invention provides the hindered amine compound of the first invention wherein, in the general formula (I), R is an alkyl group having 4-22 carbon atoms, n=2, and R 1 is an alkylene group having 2-12 carbon atoms.
[0015] The third invention provides the hindered amine compound of the first invention wherein, in the general formula (I), n=1, and R 1 is a group having the following general formula (III):
[0000]
[0000] (R is an alkyl group having 10-22 carbon atoms).
[0016] The fourth invention provides a synthetic resin composition wherein 0.01-10 weight parts of the hindered amine compound according to any of the first-third inventions is blended with 100 weight parts of a synthetic resin.
[0017] The fifth invention provides a polyolefin resin composition wherein 0.05-5 weight parts of the hindered amine compounds according to any of the first-third inventions is blended with 100 weight parts of a polyolefin resin.
[0018] The sixth invention provides a polyolefin film for agricultural use comprising the polyolefin resin composition according to the fifth invention.
[0019] The seventh invention provides a coating composition stabilized by the hindered amine compound according to any of the first-third inventions.
[0020] The eighth invention provides a synthetic resin composition wherein 1-30 weight parts of one or more of melamine phosphate, melamine pyrophosphate, melamine polyphosphate, piperazine phosphate, piperazine pyrophosphate and piperazine polyphosphate as a flame retarder, and 0.01-10 weight parts of the hindered amine compound according to any of the first-third inventions, is blended with 100 weight parts of a synthetic resin.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0021] Some preferred aspects of the invention will now be described.
[0022] The hindered amine compound of the present invention is a weakly basic hindered amine compound having a carbonate skeleton represented by the general formula (I) or (II).
[0023] Examples of an alkyl group having 1-30 carbon atoms represented by R in the general formulae (I) and (II), are linear- or branched-alkyl groups such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, pentyl, sec-pentyl, tert-pentyl, hexyl, heptyl, octyl, iso-octyl, 2-ethylhexyl, tert-octyl, nonyl, isononyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl and octadecyl, and cycloalkyl groups such as cyclohexyl.
[0024] Examples of a hydroxyalkyl group having 1-30 carbon atoms represented by R in the general formulae (I) and (II), are 2-hydroxyethyl, 2-hydroxypropyl, 2-hydroxybutyl and 2-hydroxy-2-methylpropyl.
[0025] R may be identical or different every n repeating units.
[0026] Examples of an alkenyl group having 2-30 carbon atoms represented by R in the general formulae (I) and (II) are alkenyl groups corresponding to the aforesaid alkyl groups such as vinyl, allyl, butenyl, pentenyl and oleyl.
[0027] In the general formula (I), when n=1, R 1 is an alkyl group having 1-22 carbon atoms, an alkenyl group having 2-22 carbon atoms, or a group having the aforesaid general formula (III).
[0028] In the general formula (I), when n=1, examples of an alkyl group having 1-22 carbon atoms represented by R 1 are methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, pentyl, sec-pentyl, tert-pentyl, hexyl, heptyl, octyl, iso-octyl, 2-ethylhexyl, tert-octyl, nonyl, isononyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl and behenyl.
[0029] In the general formula (I), when n=1, examples of an alkenyl group having 2-22 carbon atoms represented by R 1 are alkenyl groups corresponding to the aforesaid alkyl groups such as vinyl, allyl, butenyl, pentenyl and oleyl.
[0030] In the general formula (I), when n=1, and R 1 is a group having the aforesaid general formula (III), an example of R in the general formula (III) is identical to R in the general formula (I), but it may be identical to or different from R in the general formula (I).
[0031] R is preferably an alkyl group having 10-22 carbon atoms.
[0032] In the general formula (I), when n=2-6, examples of an organic group having 2-20 carbon atoms of valency n represented by R 1 are residues other than the hydroxyl group of a multivalent hydroxyl compound of valency n.
[0033] Examples of the aforesaid multivalent hydroxyl compound are ethylene glycol, propylene glycol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, neopentylglycol, 1,6-hexanediol, 1,3-cyclohexanediol, 1,4-cyclohexanediol, bisphenol A hydrate, bisphenol F hydrate, diethylene glycol, triethylene glycol, glycerol, trimethylol propane, pentaerythritol, and dip entaerythritol.
[0034] In the general formula (II), R 2 is a hydrogen atom, an alkyl group having 1-22 carbon atoms, or an alkenyl group having 2-22 carbon atoms.
[0035] Examples of an alkyl group having 1-22 carbon atoms represented by R 2 , are the alkyl groups in the aforesaid R having this number of carbon atoms.
[0036] Examples of an alkenyl group having 2-22 carbon atoms represented by R 2 in the general formula (II), are the alkenyl groups in the aforesaid R having this number of carbon atoms.
[0037] R 2 may be the same or may differ every n repeating units. In the general formula (II), A represents a single bond, a linear- or branched-alkylene group having 1-12 carbon atoms, or an alkylene group with an ether linkage.
[0038] Examples of an alkylene group having 1-12 carbon atoms represented by A are methylene, 1,2-ethylene, 1,2-propylene, 1,3-propylene, tetramethylene, 1,2-butylene, 1,3-butylene, pentamethylene, 2,2-dimethyltrimethylene, hexamethylene and octamethylene.
[0039] Examples of a linear- or branched-alkylene group having 1-12 carbon atoms with an ether linkage represented by A in the general formula (II), are:
[0000] —CH 2 CH 2 O—CH 2 CH 2 —,
[0000] —CH 2 CH(CH 3 )—O—CH 2 CH(CH 3 )—, and
[0000] —CH 2 CH 2 —O—CH 2 CH 2 —O—CH 2 CH 2 —.
[0040] A may be the same or different every n repeating units (n=2-6).
[0041] In the general formula (II), X is —C(═O)—, a linear- or branched-alkylene group having 4-40 carbon atoms with a terminal —C(═O)O—, a linear- or branched-alkylene group having 4-40 carbon atoms with a carbonic acid ester linkage, or an organic group having 6-30 carbon atoms with 3-6 terminal —O—C(═O)—.
[0042] In the general formula (II), an example of an alkylene group having 4-40 carbon atoms with a terminal —C(═O)O— represented by X, is:
[0000] —C(═O)—O—(CH 2 ) p —O—C(═O)—
[0043] In the general formula (II), an example of an alkylene group having a carbonic acid ester linkage represented by X, is:
[0000] —C(═O)—R 3 —O—C(═O)—O—R 3 —C(═O)—
[0000] (where p is a number from 2-40, and R 3 is an alkylene group having 2-18 carbon atoms).
[0044] In the general formula (II), examples of an organic group having 3-6 terminal —O—C(═O)— represented by X, are:
[0000]
[0045] More specifically, examples of a compound represented by the general formula (I) are Compounds No. 1-No. 6 and Compound No. 13, and examples of a compound represented by the general formula (II) are Compounds No. 7-No. 12. However, the invention is not to be construed as being limited in any way by the following compounds:
[0000]
[0046] The method of synthesizing the compound represented by the general formula (I) is not particularly limited, but it may be synthesized by the methods usually used for organic synthesis shown in the Examples described later, and it may be purified by distillation, recrystallization, re-precipitation, a filter medium or an adsorbent as required.
[0047] Examples of the synthetic resin stabilized by the hindered amine compound represented by the general formula (I), are homopolymers or copolymers of α-olefins such as polypropylene, low density polyethylene, linear low density polyethylene, high density polyethylene, polybutene-1, poly-3-methylpentene, poly-4-methylpentene and ethylene-propylene copolymer; copolymers of α-olefins with polyunsaturated compounds such as conjugated dienes or unconjugated dienes; copolymers of α-olefinss with acrylic acid, methacrylic acid, vinylacetate etc.; linear polyesters or acid-modified polyesters such as polyethylene terephthalate, polyethylene terephthalate isophthalate, polyethylene p-oxybenzoate and polybutylene terephthalate; aliphatic polyesters having biodegradability such as polylactic acid; polyamides such as polycaprolactam and polyhexamethylene adipamide; polyimides; polystyrenes and copolymers of styrene and/or α-methylstyrene with other monomers (e.g., maleic anhydride, phenyl maleimide, methyl methacrylate, butadiene, acrylonitrile) (e.g., AS resin, ABS resin, MBS resin, heat-resistant ABS resin); halogen containing resin such as polyvinyl chloride, polyvinylidene chloride, polyethylene chloride, polypropylene chloride, polyvinylidene fluoride, chlorinated rubber, vinyl chloride-vinyl acetate copolymer, vinyl chloride-ethylene copolymer, vinyl chloride-vinylidene chloride copolymer, vinyl chloride-vinylidene chloride-vinyl acetate terpolymer, vinyl chloride-acrylic ester copolymer, vinyl chloride-maleic acid ester copolymer and vinyl chloride-cyclohexyl maleimide copolymer; polymers of (meth)acrylic acid esters such as methyl(meth)acrylate, ethyl(meth)acrylate and octyl(meth)acrylate; polyether ketone, polyvinyl acetate, polyvinyl formal, polyvinyl butyral and polyvinyl alcohol; linear- or branched-polycarbonates, petroleum resin, cumarone resin, polyphenylene oxide, polyphenylene sulfide, polyurethane, thermoplastic resins such as cellulose resins; thermosetting resins such as epoxy resin, phenol resin, urea resin, melamine resin and unsaturated polyester resins; elastomers such as isoprene rubber, butadiene rubber, butadiene-styrene copolymer rubber, butadiene-acrylonitrile copolymer rubber, acrylonitrile-butadiene-styrene copolymer rubber, and copolymer rubbers with α-olefins such as ethylene, propylene and butane-1, and terpolymer rubbers of ethylene-α-olefins with unconjugated dienes such as ethylidene norbornene and cyclopentadiene; cyclo-olefin copolymers; and silicone resins. These resins and/or elastomers may be alloyed or blended together.
[0048] Preferably, it is a polyolefin resin.
[0049] The stabilizing effect on this synthetic resin differs according to the degree of stereoregularity, specific gravity, type of polymerization catalyst in the polyolefin such as a Ziegler-Natta catalyst or metallocene catalyst, whether or not the polymerization catalyst is removed and to what extent, degree of crystallization, polymerization conditions such as temperature and pressure, type of crystals, size of lamellar crystals measured by X-ray small angle scattering, the aspect ratio of crystals, solubility in aromatic or aliphatic solvents, solution viscosity, melt viscosity, average molecular weight, extent of molecular weight distribution, number of peaks in the molecular weight distribution, whether it is a block or random copolymer and the blending ratio of each monomer, but any of the aforesaid resins may be used.
[0050] The hindered amine compound of the invention is used for various shaping starting materials in a synthetic resin composition wherein 0.01-10 weight parts, and preferably 0.05-5 weight parts, is blended with 100 weight parts of the aforesaid synthetic resin.
[0051] If the blending amount of the hindered amine compound is too much below than the aforesaid range, there is no stabilization effect, whereas if it is too much above the aforesaid range, no additional effect can be expected and there is a risk that the physical properties of the resin will be impaired.
[0052] In particular, in the case of a polyolefin resin, 0.05-5 weight parts and preferably 0.1-3 weight parts of the hindered amine compound is blended with 100 weight parts of the polyolefin resin.
[0053] The method of blending the hindered amine compound represented by the general formula (1) is not particularly limited, and may be any technique for blending a stabilizer with a resin known in the art. For example, it may be added to the polymerization system before the synthetic resin is polymerized, added during polymerization, or added after polymerization. If it is to be added after polymerization, a powder of the resin, pellets or the mixture from a Henschel mixer may be kneaded in an extruder or the like, sprayed as a solution to impregnate the synthetic resin, or used after making up a master batch. The type of processing machine, processing temperature and cooling conditions after processing are not particularly limited, but the conditions are preferably selected so that the physical properties of the resin suit the envisaged application. The hindered amine compound of the invention may also be formed into particles, either alone or with another additive.
[0054] When using the hindered amine compound represented by the general formula (I) of the present invention for stabilizing a synthetic resin or coating material, various kinds of blending agents usually used for resins may be employed as required. Examples of such blending agents are a phenol type antioxidant, sulfur type antioxidant, phosphorus type antioxidant, ultraviolet absorber, another hindered amine compound, nucleating agent, flame retarder, flame retarder auxiliary agent, lubricant, filler, plasticizer, fibrous filler, metal soap, hydrotalcite, antistatic agent, pigment, dye, antibacterial agent, anti-mold agent, antiseptic, stain-proofing agent, anticorrosive, surfactant, compatibilizer, sedimentation inhibitor, polymerization inhibitor, thickener, defoaming agent, coupling agent, leveling agent, drying agent, anti-creasing agent, dehydrating agent, curing catalyst, adhesion imparting agent and foaming agent.
[0055] Examples of a phenol type antioxidant are α-tocopherol, 2,6-di-t-butyl-p-cresol, 2,6-diphenyl-4-octadecyloxyphenol, distearyl(3,5-di-t-butyl-4-hydroxybenzyl)phosphonate, 1,6-hexamethylene bis[(3,5-di-t-butyl-4-hydroxyphenyl) propionic acid amide], 4,4′-thiobis (6-t-butyl-m-cresol), 2,2′-methylene bis(4-methyl-6-t-butylphenol), 2,2′-methylene bis(4-ethyl-6-t-butylphenol), 4,4′-butylidene bis(6-t-butyl-m-cresol), 2,2′-ethylidene bis(4,6-di-t-butylphenol), 2,2′-ethylidene bis(4-s-butyl-6-t-butylphenol), 1,1,3-tris(2-methyl-4-hydroxy-5-t-butylphenyl)butane, 1,3,5-tris(2,6-dimethyl-3-hydroxy-4-t-butylbenzyl)isocyanurate, 1,3,5-tris(3,5-di-t-butyl-4-hydroxybenzyl)isocyanurate, 1,3,5-tris(3,5-di-t-butyl-4-hydroxybenzyl)-2,4,6-trimethylbenzene, 2-t-butyl-4-methyl-6-(2-acryloyloxy-3-t-butyl-5-methylbenzyl)phenol, stearyl (3,5-di-t-butyl-4-hydroxyphenyl) propionate, thiodiethyleneglycol bis[(3,5-di-t-butyl-4-hydroxyphenyl)propionate], 1,6-hexamethylene bis-(3,5-di-t-butyl-4-hydroxyphenyl)propionate], bis[3,3-bis(4-hydroxy-3-t-butylphenyl)butyric acid]glycolester, bis[2-t-butyl-4-methyl-6-(2-hydroxy-3-t-butyl-5-methylbenzyl)phenyl]terephthalate, 1,3,5-tris[(3,5-di-t-butyl-4-hydroxyphenyl)propionyl oxyethyl]isocyanurate, 3,9-bis[1,1-dimethyl-2{(3-t-butyl-4-hydroxy-5-methylphenyl)propionyloxy}ethyl]2,4,8,10-tetraoxaspiro[5.5]undecane and triethyleneglycol bis[(3-t-butyl-4-hydroxy-5-methylphenyl)propionate].
[0056] Examples of a sulfur type antioxidant are dialkyl thiodipropionates such as dilauryl thiodipropionate, dimyristyl thiodipropionate and distearyl thiodipropionate, and β-alkyl mercaptopropionic acid esters of polyols such as pentaerythritol tetra(β-dodecyl mercaptopropionate).
[0057] Examples of a phosphorus type antioxidant are tris-nonyl phenylphosphite, tris[2-t-butyl-4-(3-t-butyl-4-hydroxy-5-methylphenylthio)-5-methylphenyl]phosphite, tridecyl phosphite, octyl diphenyl phosphite, di(decyl)monophenyl phosphite, di(tridecyl)pentaerythritol diphosphite, di(nonylphenyl)pentaerythritol diphosphite, bis(2,4-di-t-butylphenyl) pentaerythritol diphosphite, bis(2,6-di-t-butyl-4-methylphenyl) pentaerythritol diphosphite, bis(2,4,6-tri-t-butylphenyl)pentaerythritol diphosphite, bis(2,4-dicumylphenyl)pentaerythritoldiphosphite, tetra(tridecyl) isopropylidene diphenoldiphosphite, tetra(tridecyl)-4,4′-n-butylidene bis(2-t-butyl-5-methylphenol)diphosphite, hexa(tridecyl)-1,1,3-tris(2-methyl-4-hydroxy-5-t-butylphenyl)butanetriphosphite, tetrakis(2,4-di-t-butylphenyl)biphenylene diphosphonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2,2′-methylene bis(4,6-t-butylphenyl)-2-ethylhexylphosphite, 2,2′-methylene bis(4,6-t-butylphenyl)-octadecylphosphite, 2,2′-ethylidene bis(4,6-di-t-butylphenyl)fluorophosphite, tris(2-[(2,4,8,10-tetrakis-t-butyldibenzo[d,f][1,3,2]dioxaphosphepine-6-il)oxy]ethyl)amine, and the phosphites of 2-ethyl-2-butyl propyleneglycol and 2,4,6-tri-t-butylphenol.
[0058] The aforesaid phenol type, sulfur type and phosphorus type antioxidant may be used alone or together, in which case their total amount is 0.001-10 weight parts, or more preferably, 0.05-5 weight parts relative to 100 weight parts of resin.
[0059] Examples of an aforesaid ultraviolet absorber are 2-hydroxybenzophenones such as 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-octoxybenzophenone, 5,5′-methylene bis(2-hydroxy-4-methoxybenzophenone); 2-(2′-hydroxyphenyl)benzotriazoles such as 2-(2′-hydroxy-5′-methylphenyl)benzotriazole, 2-(2′-hydroxy-3′,5′-di-t-butylphenyl)-5-chlorobenzotriazole, 2-(2′-hydroxy-3′-t-butyl-5′-methylphenyl)-5-chlorobenzotriazole, 2-(2′-hydroxy-5′-t-octylphenyl)benzotriazole, 2-(2′-hydroxy-3′,5′-dicumylphenyl)benzotriazole and 2-(2′-hydroxy-3′-t-butyl-5′-carboxyphenyl)benzotriazole; benzoates such as phenyl salicylate, resorcinol monobenzoate, 2,4-di-t-butylphenyl-3,5-di-t-butyl-4-hydroxybenzoate, 2,4-di-t-amylphenyl-3,5-di-t-butyl-4-hydroxybenzoate and hexadecyl-3,5-di-t-butyl-4-hydroxybenzoate; substituted oxanilides such as 2-ethyl-2′-ethoxyoxanilide and 2-ethoxy-4′-dodecyloxanilide; cyanoacrylates such as ethyl-α-cyano-β, β-diphenylacrylate and methyl-2-cyano-3-methyl-3-(p-methoxyphenyl)acrylate; and triallyl triazines such as 2-(2-hydroxy-4-octoxyphenyl)-4,6-bis (2,4-di-t-butylphenyl)-s-triazine, 2-(2-hydroxy-4-methoxyphenyl)-4,6-diphenyl-s-triazine and 2-(2-hydroxy-4-propoxy-5-methylphenyl)-4,6-bis(2,4-di-t-butylphenyl)-s-triazine. These are used in the amount of 0.001-10 weight parts, but more preferably 0.05-5 weight parts, relative to 100 weight parts of resin.
[0060] Examples of the other hindered amine compound mentioned above, are 2,2,6,6-tetramethyl-4-piperidyl-1-oxy-, 2,2,6,6-tetramethyl-4-piperidyl stearate, 1,2,2,6,6-pentamethyl-4-piperidyl stearate, 2,2,6,6-tetramethyl-4-piperidyl benzoate, bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate, bis(1,2,2,6,6-pentamethyl-4-piperidyl)sebacate, tetrakis(2,2,6,6-tetra-methyl-4-piperidylbutane)tetracarboxylate, tetrakis(1,2,2,6,6-pentamethyl-4-piperidylbutane)tetracarboxylate, bis(2,2,6,6-tetramethyl-4-piperidyl)-di(tridecyl)-1,2,3,4-butanetetracarboxylate, bis(1,2,2,6,6-pentamethyl-4-piperidyl)-di(tridecyl)-1,2,3,4-butanetetracarboxylate, bis(1,2,2,6,6-pentamethyl-4-piperidyl)-2-butyl-2-(3,5-di-t-butyl-4-hydroxybenzyl) malonate, 1-(2-hydroxyethyl)-2,2,6,6-tetramethyl-4-piperidinol/diethylsuccinate condensation polymer, 1,6-bis(2,2,6,6-tetramethyl-4-piperidylamino) hexane/dibromoethane condensation polymer, 1,6-bis (2,2,6,6-tetramethyl-4-piperidylamino) hexane/2,4-dichloro-6-morpholino-s-triazine condensation polymer, 1,6-bis(2,2,6,6-tetramethyl-4-piperidylamino) hexane/2,4-dichloro-6-t-octylamino-s-triazine condensation polymer, 1,5,8,12-tetrakis[2,4-bis (N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino)-s-triazine-6-il]-1,5,8,12-tetraazadodecane, 1,5,8,12-tetrakis[2,4-bis(N-butyl-N-(1,2,2,6,6-pentamethyl-4-piperidyl)amino)-s-triazine-6-il]-1,5,8,12-tetraazadodecane, 1,6,11-tris[2,4-bis(N-butyl-N-(2,2,6,6-tetramethyl-4-piperidyl)amino)-s-triazine-6-il-amino]undecane and 1,6,11-tris[2,4-bis(N-butyl-N-(1,2,2,6,6-pentamethyl-4-piperidyl) amino)-s-triazine-6-il amino]undecane.
[0061] Examples of a nucleating agent are aromatic carboxylic acid metal salts such as aluminum p-t-butyl benzoate and sodium benzoate; acid phosphoric acid ester metal salts such as bis(2,4-di-t-butylphenyl) sodium phosphate, bis(2,4-di-t-butylphenyl) lithium phosphate and sodium-2,2′-methylene bis(4,6-di-t-butylphenyl) phosphate; and polyhydric alcohol derivatives such as dibenzylidene sorbitol and bis(methylbenzylidene) sorbitol.
[0062] Examples of a flame retarder are halogen type flame retarders, phosphorus type flame retarders such as red phosphorus, melamine phosphate, piperazine phosphate, guanidine phosphate, melamine pyrophosphate, piperazine pyrophosphate, guanidine pyrophosphate, melamine polyphosphate, melamine polyphosphate, guanidine polyphosphate, phosphoric acid ester compounds and phosphazene compounds, nitrogen type flame retarders such as melamine cyanurate, and metal hydroxides such as magnesium hydroxide and aluminum hydroxide; examples of a flame retarder auxiliary agent are inorganic compounds such as antimony trioxide and zinc borate, and drip inhibitors such as polytetrafluoroethylene.
[0063] The hydrotalcite may be a natural product or a synthetic compound, and it may be used regardless of whether or not a surface treatment has been performed, or whether or not it has any water of crystallization. For example, the basic carbonate represented by the following general formula (IV) may be mentioned.
[0000] M x Mg y Al z CO 3 (OH) xp+2y+3z−2 .n H 2 0 (IV)
[0000] (in the formula, M is an alkali metal or zinc, X is a number from 0-6, y is a number from 0-6, z is a number from 0.1-4, p is the valency of M, and n represents the number of molecules of water of crystallization from 0-100.
[0064] An example of a lubricant are fatty acid amides such as lauryl amide, myristyl amide, lauryl amide, stearyl amide and behenyl amide, ethylene bis-stearyl amide, polyethylene wax, metal soaps such as calcium stearate and magnesium stearate, and metal salts of phosphoric acid esters such as magnesium distearyl phosphoric acid ester and magnesium stearyl phosphoric acid ester.
[0065] Examples of a filler are an inorganic material such as talc, silica, calcium carbonate, glass fiber, potassium titanate, potassium borate, carbon black or carbon fiber, carbon nanoparticles such as fullerene and carbon nanotube. When the inorganic material consists of spherical particles, the particle size may be selected as appropriate. When it consists of fibers, the fiber diameter, fiber length and aspect ratio may be selected as appropriate. The filler may also be given a surface treatment if required.
[0066] When the resin composition with which the hindered amine compound of the present invention was blended, is used as an agricultural film, an ultraviolet absorber may be blended therewith to control the growth of crops, an infrared absorption agent may be blended therewith to improve temperature retention properties, and since fogging may occur in a greenhouse, and condensation may form on the film surface which prevents sufficient light from reaching the crops, an anti-clouding agent, anti-misting agent or drop-flowing agent may also be blended therewith.
[0067] The hindered amine compound of this invention has the effect of stabilizing a synthetic resin, and in particular, the synthetic resin composition may be used as a polyolefin agricultural film exposed to acidic components by the fumigation of agricultural chemicals or sulfur, a coating material exposed to acid rain outdoors, or a sealant.
[0068] The hindered amine compound of the present invention may also be used in applications in which a long-term stabilization effect of an organic substance is required, such as resin compositions having acidic ingredients in which the prior art hindered amine compounds were not fully able to demonstrate a stabilization effect due to the effect of the acidic ingredients such as melamine pyrophosphate, liquid products such as lubricating oils or electrolytic solutions.
EXAMPLES
[0069] The invention will now be described in detail referring to specific examples, but the invention is not to be construed as being limited in any way by the following Examples.
Example 1
Synthesis of Compound No. 1
[0070] 17.0 g (98.1 mmol) of 4-hydroxy-1-oxy-2,2,6,6-tetramethyl piperidine was dissolved in 40.0 g of chlorobenzene, and a solution containing 31.3 g (78.5 mmol) dilauroyl peroxide dissolved in 125 g chlorobenzene was dripped in at 70° C. over 3 hours. The reaction was performed at this temperature for a further 6 hours. The obtained reaction liquid was analyzed by gas chromatography to verify consumption of the starting materials. The obtained reaction liquid was a mixture of 4-hydroxy-1-undecanoxy-2,2,6,6-tetramethyl piperidine, 1-undecanoxy-2,2,6,6-tetramethyl piperidine-4-one, lauric acid and a solvent. 50 g of hexane was added to the reaction liquor, the reaction liquor was washed with 53.9 g (98 mmol) of 7.3% sodium hydroxide aqueous solution and 25 g methanol, washed twice more with 30 g water, and lauric acid was removed. The mixture was dried with anhydrous magnesium sullfate, the magnesium sulfate was removed by filtration, and the solvent was removed under reduced pressure on the evaporator. 70 ml of ethanol was added to the concentrate, and 20 ml of an ethanol solution of 0.57 g (15 mmol) of sodium borohydride was dripped in at room temperature for 20 minutes. The mixture was reacted for a further 1 hour, elimination of 1-undecanoxy-2,2,6,6-tetramethyl piperidine-4-one was verified, the solvent removed under reduced pressure, 50 ml of toluene was added, and the mixture washed 5 times with 30 ml water. Next, water was removed by evaporation under reduced pressure with reflux at 40° C., the solvent was removed under reduced pressure, and 23.0 g of 4-hydroxy-1-undecanoxy-2,2,6,6-tetramethyl piperidine of purity 96.1% as determined by area ratio on the gas chromatograph, was obtained as a colorless liquid (yield 68.8%).
[0071] 12.0 g (35.17 mmol) of the obtained 4-hydroxy-1-undecanoxy-2,2,6,6-tetramethyl piperidine of purity 96.1%, 4.19 g (19.34 mmol) of diphenyl carbonate and 0.6 g of potassium carbonate were dispersed in 100 ml of mineral spirits, reacted at 170-180° C. for 8 hours, and phenol was removed. The mixture was cooled to 40° C., and washed 3 times with 30 ml water. Water was removed by evaporation under reduced pressure with reflux at 60° C., and the solvent was removed under reduced pressure on the evaporator. The concentrate was purified by silica gel column chromatography (developing solvent: toluene), and bis(1-undecanoxy-2,2,6,6-tetramethyl piperidine-4-il) carbonate (yield 55.5%) of purity 99.9% by the aforesaid analysis method was obtained as a colorless liquid.
[0072] The analysis result of the obtained Compound No. 1 is shown below:
IR Spectrum
[0073] 2800-3050 cm −1 , 1740 cm −1 , 1450 cm −1 , 1380 cm −1 , 1360 cm −1 , 1310 cm −1 , 1270 cm −1 , 1240 cm −1 , 1190 cm −1 , 1000 cm −1
[0074] 1 H-NMR spectrum (H: Actual measurement of number of protons, figures in brackets [ ] are calculated values)
δ 0.75-2.05 (H in CH 3 and C—CH 2 —C, 72.8 [74])
δ 3.55-3.85 (H in CH 2 —O: 4.2 [4])
δ 4.60-5.10 (H in CH—O: 2.0 [2])
Example 2
Synthesis of Compound No. 7
Synthesis of 1-undecaneoxy-2,2,6,6-tetramethyl piperidine-4-one
[0075] 15.0 g (86.6 mmol) of 4-hydroxy-1-oxy-2,2,6,6-tetramethyl piperidine was dissolved in 40.0 g of chlorobenzene, and a solution containing 27.6 g (69.3 mmol) dilauroyl peroxide dissolved in 125 g chlorobenzene was dripped in at 70° C. over 3 hours. The reaction was performed at this temperature for a further 6 hours. The obtained reaction liquid was analyzed by gas chromatography to verify consumption of the starting materials. 0.1 g of 4-acetyl-1-oxy-2,2,6,6-tetramethyl piperidine was added to the reaction liquor to suppress decomposition reactions, the mixture was cooled to 0° C., and 48.3 g (64.9 mmol) of 10% sodium hypochlorite aqueous solution was dripped in over 3 hours. The reaction was continued for 3 hours at the same temperature, 15 ml of 15 wt % sodium thiosulfate aqueous solution was added, and the mixture was heated to 40° C. and reacted for 1 hour. The organic layer and aqueous layer were separated, the aqueous layer was extracted twice with 70 ml toluene, and the toluene was dehydrated by anhydrous magnesium sulfate together with the organic layer. The magnesium sulfate was filtered off, the filtrate was concentrated under reduced pressure, 50 g hexane was added, 17.3 g (86.6 mmol) of 20% sodium hydroxide aqueous solution was added at 55° C., 15 g methanol was added, and the mixture allowed to stand. The aqueous layer was removed, and washed twice with 15 g water. The water was removed by heating under reflux, the solvent was removed, the mixture dissolved in 40 g methanol, cooled to 40° C., and crystals were deposited. 14.4 g of a white powder of 1-undecyloxy-2,2,6,6-tetramethyl piperidine-4-one was obtained by filtration (yield 50%). It was a colorless liquid at room temperature.
[0076] The analysis result of the obtained Compound No. 7 is shown below.
IR Spectrum
[0077] 2860-3040 cm −1 , 2360 cm −1 , 1740 cm −1 , 1460 cm −1 , 1360 cm −1 , 1265 cm −1 , 1200 cm −1 , 1100 cm −1 , 980 cm −1
[0078] 1 H-NMR spectrum (H: Actual measurement of number of protons, figures in brackets [ ] are calculated values.)
δ 0.75-2.10 (H in CH 3 and C—CH 2 —C, 85.4 [84])
δ 3.25-4.45 (H in CH 2 —O: 16.0 [16])
Synthesis of Cyclic-Acetal Skeleton Intermediate
Synthesis Example 1 and Synthesis Example 2
[0079] 8.00 g (24.58 mmol) of 1-undecanoxy-2,2,6,6-tetramethyl piperidine-4-one, (34.41 mmol) of the polyhydric alcohol shown in TABLE 1, 0.54 g of p-toluene sulfonic acid and 76.00 g cyclohexane were introduced into a flask, 25 g methanol was dripped in at 70-80° C. over 7 hours, and the mixture was kept at the same temperature for a further 2 hours. Methanol and water were distilled off, the mixture was cooled to 40° C., 40 ml of ethyl acetate, 0.15 g of sodium carbonate and 30 ml of water were added, and the mixture stirred for 30 minutes. After standing, the aqueous layer was removed, washed twice more with 20 ml water, the organic layer was dried with anhydrous magnesium sulfate, and the magnesium sulfate was removed by filtration. The filtrate was evaporated under reduced pressure, and a light yellow, viscous liquid was obtained. The obtained liquid was purified by column chromatography (silica gel). TABLE 1 shows the diol used, yield, description and purity measured by liquid chromatography.
[0080] The compound obtained in Synthesis Example 1 is an intermediate of Compound No. 7, and the compound obtained in Synthesis Example 2 was used for Example 3 as an intermediate of Compound No. 11.
[0000]
TABLE 1
Synthesis
Yield
Description
Purity
Example
Polyvalent alcohol
(%)
(Liquid)
(%)
1
Trimethyloylpropane
80.6
Light yellow
99.9
2
Glycerine
63.7
Light yellow
99.9
[0081] 8.10 g (18.4 mmol) of 1,5-dioxa-9-aza-3-ethyl-3-hydroxymethyl-8,8,10,10-tetramethyl-9-undecyloxyspiro[5.5]undecane, 2.16 g (10.1 mmol) diphenyl carbonate and 0.7 g of potassium carbonate were dispersed in 100 ml of mineral spirit, reacted at 170-180° C. for 8 hours, and phenol was removed. The mixture was cooled to 40° C., and washed 3 times with 30 ml water. Water was removed under reduced pressure with reflux at 60° C., and the solvent was removed under reduced pressure on the evaporator. The concentrate was recrystallized from ethanol by cooling to 0° C., and Compound No. 7 of purity 99.3% (yield 39.5%) was obtained as colorless crystals with a melting point of 118.8° C.
Example 3
Synthesis of Compound No. 11
[0082] 8.0 g (20 mmol) of the 1,5-dioxa-9-aza-3-hydroxy-8,8,10,10-tetramethyl-9-undecyloxyspiro[5.5]undecane obtained in Synthesis Example 2, 2.35 g (11.0 mmol) diphenyl carbonate and 0.7 g potassium carbonate were dispersed in 100 ml mineral spirit, reacted at 170-180° C. for 8 hours, and phenol was removed. The mixture was cooled to 40° C., and washed 3 times with 30 ml water. Water was removed under reduced pressure with reflux at 60° C., and the solvent was removed under reduced pressure on the evaporator. The concentrate was recrystallized from ethanol by cooling to 0° C., and Compound No. 11 of purity 99.9% was obtained as colorless crystals with a melting point of 87.4° C. (yield 68.4%).
[0083] The analysis result of the obtained compound No. 11 is shown below.
IR Spectrum
[0084] 2850-2920 cm −1 , 1750 cm −1 , 1470 cm −1 , 1360 cm −1 , 1280 cm −1 , 1230 cm −1 , 1200 cm −1 , 1100 cm −1 , 1030 cm −1 , 960 cm −1 .
[0085] 1 H-NMR spectrum (H: Actual measurement of number of protons, figures in brackets [ ] are calculated values.)
δ 0.75-2.05 (H in CH 3 and C—CH 2 —C, 76.2 [74])
δ 3.60-4.70 (H in CH 2 —O and CH—O: 14.0 [14])
Example 4
Synthesis of Compound No. 13
[0086] 10.0 g (57.7 mmol) of 4-hydroxy-1-oxy-2,2,6,6-tetramethylpiperidine was dissolved in 40.0 g chlorobenzene, and a solution of 54.4 g (49.1 mmol) distearoyl peroxide dissolved in 200 g chlorobenzene was dripped in at 70° C. over 2 hours. The reaction was continued for a further 3 hours at the same temperature, and the obtained reaction liquor was analyzed by gas chromatography. The area ratio of starting material:stearic acid:target material was 7.8:21.9:70.3. Solvent was removed from the reaction liquor under reduced pressure, 40 g hexane was added, 31.6 g (57.7 mmol) of 7.3% sodium hydroxide aqueous solution and 25 g ethanol were added, the mixture stirred at 40° C. for 30 minutes, washed by oil/water separation, washed twice more with 30 g water, and lauric acid was removed. The mixture was dried with anhydrous magnesium sulfate, the magnesium sulfate was removed by filtration, and the solvent was removed under reduced pressure on the evaporator. 40 ml of ethanol was added to the concentrate, and 0.19 g (5 mmol) of sodium borohydride dissolved in 5 ml ethanol was dripped in at room temperature for 10 minutes. The mixture was reacted for a further 1 hour, elimination of 1-undecanoxy-2,2,6,6-tetramethylpiperidine-4-one was verified, the solvent removed under reduced pressure, 40 ml of toluene was added, and the mixture washed 5 times with 20 ml water. Next, water was removed by evaporation under reduced pressure with reflux at 40° C., the solvent was removed under reduced pressure, the mixture, as 40 ml of an ethanol solution at 40° C., was cooled to 0° C., and 4-hydroxy-1-stearyloxy-2,2,6,6-tetramethylpiperidine of purity 94.0% as determined by area ratio on the gas chromatograph, was obtained as white crystals (yield 26.4%).
[0087] 8.70 g (19.9 mmol) of the obtained 4-hydroxy-1-stearyloxy-2,2,6,6-tetramethylpiperidine, 2.15 g (9.90 mmol) of diphenyl carbonate and 0.2 g of potassium carbonate were dispersed in 60 ml of mineral spirits, reacted at 170-180° C. for 6 hours, and phenol was removed. The mixture was cooled to 50° C., and washed 3 times with 30 ml water. Water was removed by evaporation under reduced pressure with reflux at 60° C., and the solvent was removed under reduced pressure on the evaporator. The concentrate was crystallized from a mixed solvent (toluene/ethanol=2:8 (volume ratio)), and bis(1-stearyloxy-2,2,6,6-tetramethylpiperidine-4-il) carbonate (yield 73.8%) of purity 99.9% was obtained as a white powder of melting point 52° C.
Examples 5-7 and Comparative Examples 1-4
Polyethylene Composition
[0088] 0.05 weight parts of calcium stearate, 0.05 weight parts of tetrakis(3-(3,5-di-t-butyl-4-hydroxyphenyl) propionyloxymethyl)methane, 0.05 weight parts of tris(2,4-di-t-butylphenyl) phosphite and the hindered amine compound shown in TABLE 2 (weight parts) were added to 100 weight parts of linear low-density polyethylene resin (Produced by Nippon Unica Co., Ltd.: PES120), and pelletized by a single screw extruder at a cylinder temperature of 200° C. and screw rotation speed of 25 rpm. The obtained pellets were pressed at 180° C. to form a film of thickness 80 nm.
[0089] The obtained film was placed in a 1 m×1 m×1 m corrugated paper container, fumigated with 2 g of sulfur by a hot plate, left for 24 hours, and the carbonyl index was measured after exposure of 600 hours with a Sunshine Weather Meter at 63° C. under rainy conditions. Here, the carbonyl index is defined by [log(Io/I)]/d using the infrared absorption spectrum analysis data for the film. Here, Io is the transmissivity (%) before deterioration at 1710 cm −1 , I is the transmissivity (%) after deterioration, and d is the film thickness (cm). The higher the numerical value, the more the film has deteriorated. TABLE 2 shows the results.
[0000] (a) in TABLE 2 means that measurement was impossible since deterioration was too severe.
[0000]
TABLE 2
Hindered amine
Blending
Carbonyl
compound
amount
index
Example
5
Compound No. 1
0.5
0.06
6
Compound No. 7
0.5
0.30
7
Compound No. 11
0.5
0.28
Comparative
None
—
0.59
Example 1
Comparative
Comparison
Example 2
compound 1* 1
0.5
0.47
Comparative
Comparison
Example 3
compound 2* 2
0.5
(a)
Comparative
Comparison
Example 4
compound 3* 3
0.5
0.77
* 1 :
* 2 :
* 3 :
Example 8 and Comparative Example 5
[0090] 0.5 weight parts of the hindered amine compound in Table 3 was added to 100 weight parts of an organic solvent type acrylic coating (Mr. Color Super Clear: Produced by GSI Creos Co.), the mixture was coated on an aluminum substrate having a film thickness of 50-60 μm, and the gloss retention factor and color difference were measured after 500 hours exposure by a Xenon Weather Meter at 63° C. under rainy conditions (18 minutes spraying with water in 120 minutes). TABLE 3 shows the results.
[0000]
TABLE 3
Hindered amine
Gloss retention
Color
compound
(%)
difference
Example 8-1
Compound No. 1
94
6.79
Comparative
None
95
8.61
Example 5-1
Comparative
Comparison
94
10.62
Example 5-2
compound 4* 4
* 4 :
Example 9 and Comparative Example 6
[0091] 72 weight parts of a phthalic acid plasticizer (Adeka Sizer DL-911P), 10 weight parts of tricresylphospate, 3 weight parts of epoxidized soybean oil, 2.5 weight parts of a Ca/Zn liquefied stabilizer (Adeka Stub AC-212: Asahi Denka Kogyo K. K.), 0.5 weight parts of CPL-46 (liquefied perchlorate stabilizer (Adeka Stub CPL-46)), 0.83 weight parts of liquefied phosphorous acid ester stabilizer (Adeka Stub 1500: Asahi Denka Kogyo K. K.) and 0.17 weight parts of the hindered amine compound shown in TABLE 4, were blended with 100 weight parts of vinyl chloride resin (TK-1300: Shin-Etsu Chemical Industries Co., Ltd), and roll-worked into a sheet of thickness 1 mm. The weather resistance of the obtained sheet was evaluated from the color change to blackish brown by a Fade Meter at 83° C. TABLE 4 shows the results.
[0000]
TABLE 4
Hindered amine compound
Weatherability (hours)
Example 9-1
Compound No. 1
1250
Comparative
Comparison compound 2 * 2
500
Example 6-1
Comparative
Comparison compound 4 * 4
1000
Example 6-2
Example 10 and Comparative Example 7
[0092] 80 weight parts of a block polypropylene (MFR=25 g/10 minutes, density=0.9 g/cm 3 , bending elastic modulus 950 MPa), 20 weight parts of melamine pyrophosphate, 0.1 weight parts of calcium stearate, 0.1 weight parts of tetrakis(3-(3,5-di-t-butyl-4-hydroxyphenyl) propionyloxymethyl)methane, 0.1 weight parts of tris(2,4-di-t-butylphenyl) phosphite, 0.2 weight parts of polytetrafluoroethylene and 0.2 weight parts of the hindered amine compound in TABLE 5 were mixed together, and pelletized by a single screw extruder at a cylinder temperature of 230° C., and screw rotation speed of 25 rpm. The obtained pellets were injection molded at 230° C., and evaluated by a Sunshine Weather Meter at 63° C. under rainy conditions (18 minutes spraying with water in 120 minutes), and with no rain at 83° C. TABLE 5 shows the results.
[0000]
TABLE 5
Weatherability:
Weatherability:
Hindered amine
with rain
no rain
compound
(hours)
(hours)
Example 10-1
Compound No. 1
3480
960
Comparative
None
240
120
Example 7-1
Comparative
Comparison
2160
720
Example 7-2
compound 4 * 4
Example 11 and Comparative Example 8
[0093] 100 weight parts of a block polypropylene (MFR=25 g/10 minutes, density=0.9 g/cm 3 , bending elastic modulus 950 MPa), 0.1 weight parts of calcium stearate, 0.1 weight parts of tetrakis(3-(3,5-di-t-butyl-4-hydroxyphenyl) propionyloxymethyl)methane, 0.1 weight parts of tris(2,4-di-t-butylphenyl) phosphite and 0.2 weight parts of the hindered amine compound in TABLE 6 were extruded into pellets at 250° C., and injection molded at 250° C. into a test piece of thickness 2 mm. The coloring properties were evaluated from the degree of yellowing of the obtained test piece, and weatherability was evaluated by a Sunshine Weather Meter at 83° C. with no rain from the time until cracks appeared.
[0000]
TABLE 6
Heat resistance
Weatherability,
Hindered amine
(degree of
no rain
compound
yellowing)
(hours)
Example 11-1
Compound No. 1
6
1680
Comparative
None
6
240
Example 8-1
Comparative
Comparison
8.5
1320
Example 8-2
compound 4 * 4
INDUSTRIAL APPLICABILITY
[0094] Due to the present invention, a hindered amine compound which imparts long-term weather resistance can be provided. Also, a synthetic resin composition having superior long-term weather resistance, and in particular, a polyolefin resin composition suitable for agricultural films can be provided. | Hindered amines represented by the general formula (I): (wherein R is an alkyl or hydroxyalkyl group having 1 to 30 carbon atoms or alkenyl having 2 to 30 carbon atoms; n is an integer of 1 to 4; when n is 1, R 1 is alkyl having 1 to 22 carbon atoms, alkenyl having 2 to 22 carbon atoms, or a group represented by the general formula (III): (R is as defined above), while when n is 2 to 4, R 1 is an n-valent organic group having 2 to 20 carbon atoms). When added to synthetic resins or coating materials, the amines can impart long-period stabilizing effect to the resins or the materials and exhibit excellent resistance to extraction with acid rain or chemicals. | 2 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of and priority to U.S. Provisional Application Ser. No. 61/510,957, filed Jul. 22, 2011, entitled “Portable Spa Insulation,” the contents of which is incorporated by reference herein in its entirety.
BACKGROUND OF THE INVENTION
1. Field of Invention
The subject disclosure relates to portable spa construction and, more particularly, to a portable spa with improved insulation.
2. Related Art
Portable spas have become quite popular as a result of their ease of use and multiplicity of features such as varied jet and seating configurations. One area where the inventor has recognized that improvement would be desirable concerns the methods and apparatus used to insulate the spa.
SUMMARY
According to an illustrative embodiment, glass wool insulation is utilized to replace all or part of the conventional two part rigid polyurethane foam spa insulation. An illustrative method of insulating a portable spa may comprise inverting an uninsulated spa, providing a seal plate comprising a flat interior surface having at least one openable door positioned therein, lowering the sealing plate onto the bottom surface of the inverted spa, opening the door, inserting a glass wool installation apparatus into the door opening, and operating the installation apparatus to install glass wool insulation into the interior of the spa.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a portable spa placed upside down with glass wool insulation installed in the interior thereof;
FIG. 2 is a perspective view and further illustrating a blower installation tube;
FIG. 3 is a partial perspective view of an interior portion of a portable spa wherein previously installed glass wool insulation has been partially removed to expose interior spa piping;
FIG. 4 is a perspective view illustrating apparatus employed in an illustrative embodiment to install glass wool insulation in a portable spa unit;
FIG. 5 is a perspective view illustrating installation of batting material prior to blowing glass wool insulation into interior cavities of a portable spa;
FIG. 6 illustrates a typical spa firewall;
FIG. 7 is a perspective view illustrating opening of doors of a spa sealing plate according to an illustrative embodiment;
FIG. 8 is a perspective view illustrating operation of an illustrative door embodiment;
FIG. 9 is a perspective view of an illustrative embodiment of a spa door opening in an illustrative seal plate structure;
FIG. 10 is a perspective view illustrating positioning of a blower tube in a spa door opening for purposes of blowing glass wool insulation into an interior cavity of the spa;
FIG. 11 is a perspective view illustrating removal of a spa sealing plate after installation of glass wool insulation into the interior cavity of a portable spa unit;
FIG. 12 is a perspective view illustrating packing down of glass wool insulation into a spa interior after removal of the spa sealing plate; and
FIGS. 13 and 14 are perspective views illustrating attachment of a plastic bottom sheet after packing down of the glass wool insulation.
DETAILED DESCRIPTION
According to illustrative embodiments, glass wool insulation is utilized to replace all or part of conventional two part rigid polyurethane foam spa insulation. The glass wool may be, for example, the JM Spider spray-in fiberglass insulation product available from John Manville, Denver, Colo. Antistatic silicone may be added to the John Manville formula in order to eliminate static and prevent the glass wool from wicking up moisture.
In a first illustrative embodiment, a spa is positioned with its bottom end 13 up, for example, as shown in FIGS. 1-3 . A cloth or other cover may be placed over the bottom 13 of the spa 11 and fixed in position, for example, across the parallel wooden bottom rails 15 . A glass wool spraying tube 17 ( FIG. 2 ) may be then inserted through the cloth and the glass wool 16 blown into the spa interior through the tube 17 . In a production embodiment, a reusable fixture may be constructed and used to cover the spa bottom 13 during the process of blowing the glass wool 16 into the spa interior. FIG. 1 illustrates the spa 11 after insulation has been blown into several of the interior regions or cavities beneath the parallel horizontal bottom frame members or rails 15 . An advantage over rigid polyurethane foam is that the glass wool 16 may be removed in the field to facilitate repair and then replaced. FIG. 3 illustrates an area 21 where glass wool 16 has been removed to expose interior spa water piping 23 .
According to a second illustrative embodiment illustrated in FIGS. 4-14 , a spa 111 ready for insulation installment is placed upside down resting on its top rim so that glass wool insulation may be shot into it from its under or bottom side 113 . Typically, the spa 111 at this stage will comprise a spa shell 115 ( FIG. 5 ) attached to a surrounding frame 117 with exterior paneling 119 attached to the frame 117 and with all spa equipment such as pump, filter, heater, jets, and controls installed. The surrounding frame 117 may include, for example, a base frame, formed for example of perpendicularly or rectangularly arranged wooded studs 121 as shown in FIG. 4 . The spa will also typically include a “firewall” 123 ( FIG. 6 ), which, in one embodiment, may be a sheet of black corrugated polypropylene that separates the equipment compartment of the spa from the tub area, similar to the firewall in a car. Such a sheet 123 may be cut on a Numerical Controlled (NC) Router to the proper shape and to create holes, e.g. 124 , for the plumbing pipes, e.g. 125 ( FIG. 5 ), and electronics to pass through.
In a first step according to an illustrative process, illustrated in FIG. 5 , suitable batting material 127 , for example, such as polyester batting, is installed to block the firewall openings and other openings as necessary or desirable. A spray adhesive may be used to secure the batting in place. Additionally, if desired, masking tape may be used to block other small openings, and Kraft paper or other shielding may be placed around the spa exterior to protect decorative paneling 119 .
In a next step, a sealing plate 129 , shown e.g. FIGS. 4 and 7-9 , is installed by lowering it onto the spa frame members 121 . In one embodiment, this sealing plate 129 is fabricated from a flat interior sheet 131 surrounded by a rim 133 . In one embodiment, the flat sheet 131 may be attached to the rim 133 by screws or other fasteners. In one embodiment, the flat sheet 131 may be wood, such as plywood, or fiberglass, and the rim 133 may be a metal, such as, for example, aluminum. The shape of the sealing plate 129 is selected to conform to the shape of the spa bottom in illustrative embodiments.
A number of hinged doors or door “sliders” 135 are positioned on the top surface 137 of the flat sheet 131 . Each hinged door 135 is strategically positioned at a location where it is desired to inject the insulative glass wool material. In one embodiment, the doors 135 are positioned to be over the deeper parts of the spa interior in order to allow optimum filling of the spa 111 .
In one embodiment, a plate lifter 151 , e.g., FIG. 4 , comprising, for example, a chain hoist with wheels riding on a ceiling I beam or other track, may be used to suspend, mechanically lift, move and position a larger sealing plate 129 , while smaller sealing plates 129 may be handled manually. The sealing plate 129 may be placed in an initial position above the spa 111 and then aligned. In one embodiment, the alignment is by reference to locating the doors 135 over the deeper parts of the spa 111 , as mentioned above. In one embodiment shown in FIGS. 8 and 9 , a door 135 is hinged by a screw or other device 136 to pivot in the plane of the top surface 137 to reveal a rectangular opening 141 wherein is disposed a rectangular shield or membrane 143 with an “X” or other opening cut or otherwise formed in it. In one embodiment, the flexible shield 143 may be fabricated of rubber or a flexible plastic material.
Once the sealing plate 129 is in place, one of the hinged doors 135 is opened and a blower tube 155 is inserted into the opening 157 above an internal spa cavity to be filled, for example, as illustrated in FIG. 10 . The operator 159 may then employ manual assistance from other workers to hold the seal plate 127 in place against the spa unit's frame members, e.g. 121 . Of course, mechanical means may be provided in other embodiments to hold the seal plate 129 in place. Once the area beneath the blower tube 155 is visually detected to be filled, the blower 155 is turned off, and then another seal plate door 135 is opened, the blower tube 155 inserted, and the area beneath the tube 155 filled. This process is repeated for all the seal plate doors 135 until the spa's internal cavity or cavities, e.g., 130 , are completely filled.
After filling, the seal plate 129 is removed, revealing the “filled” spa unit 111 as shown in FIGS. 4 and 11-12 . The glass wool insulation 116 is then packed, pushed or tamped down by hand approximately one half inch, as shown in FIG. 12 . Any excess glass wool 116 is removed from the intake and exhaust cavities, which are the intakes for cool air to the spa's pumps and exhausts for heat from the pumps. Glass wool 116 is also removed from the top surface area of the frame member studs 121 . Any excess glass wool is also blown from the spa equipment compartment area utilizing, for example, an air hose and subsequent vacuuming.
As shown in FIGS. 13 and 14 , a sheet of plastic 161 is next placed onto the pedestal frame, centered and stapled at its edges 163 flush with the pedestal edge. In illustrative embodiments, the plastic sheet 161 may be either ABS or Polyethylene. The plastic sheet 161 seals the bottom of the spa 111 so that the glass wool insulation will not fall out. Any excess plastic around the edges 163 of the spa 111 may be trimmed off using a router or other tool.
Those skilled in the art will appreciate that various adaptations and modifications of the just described preferred embodiment can be configured without departing from the scope and spirit of the invention. Therefore, it is to be understood that, within the scope of the appended claims, the invention may be practiced other than as specifically described herein. | An uninsulated portable spa unit is inverted, and a seal plate having a flat interior surface and a plurality of doors is lowered onto the bottom surface of the inverted spa. The doors are successively opened and glass wool installation apparatus is successively inserted through the door openings and operated to install glass wool insulation into the interior of the spa unit. | 4 |
CROSS-REFERENCE TO RELATED APPLICATION
This application claims the benefit of U.S. Provisional Patent Application Ser. No. 61/122,519, filed Dec. 15, 2008; and this application is a continuation-in-part patent application of U.S. patent application Ser. No. 11/937,242, filed on Nov. 8, 2007 now U.S. Pat. No. 8,920,502, which application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/864,857, filed Nov. 8, 2006. The specifications and drawings of Ser. No. 11/937,242 and 60/864,857 are herein incorporated by reference.
FIELD OF THE INVENTION
The present invention generally relates to a vertebral body replacement to be inserted into an intervertebral space, thereby supporting the spinal column of a patient. The present invention further relates to a system and method for expanding and distracting a vertebral body replacement element into and within the spinal column of a patient.
BACKGROUND OF THE INVENTION
Back pain is one of the most significant problems facing the workforce in the United States today, is a leading cause of sickness-related absenteeism, and the main cause of disability for people between the ages of 19 and 45. Back pain can occur from pinching or irritating a spinal nerve, compression of the spine, vertebral shifting relative to the spinal cord axis, and formation of bone spurs. The most common cause of disabling back pain, however, generally stems from trauma to a vertebral disc, such as from mechanical shock, stress, tumors, or degenerative diseases. In many cases, the disc can become permanently damaged or degenerated, such that the preferred treatment necessitates partial or total excision and replacement of the damaged disc.
Traumatic injury to a vertebral disc that is not removed frequently can promote scar tissue formation. Such scar tissue typically is thicker than the healthy tissue, such that the disc continues to progressively degenerate, lose water content, and can stiffen and become significantly less effective as a shock absorber. Eventually, the disc can deform, herniate, or collapse, eliminating the flexibility of the spinal column, and potentially leading to further degeneration or damage to other vertebral discs of the spinal column. At such a point, the only option is for the damaged disc to be partially or completely removed.
When the disc is partially or completely removed, generally it is necessary to replace the excised material to prevent direct contact between the bony surfaces of the adjacent vertebrate on either side of the removed disc. For example, U.S. Pat. No. 6,824,565 of Muhanna discloses a vertebral spacer that is inserted between adjacent vertebrate to provide restorative force and function as a shock absorber between the adjacent vertebrate. Another alternative approach has been to insert a “cage” that can maintain a space occupied by the removed disc to prevent the vertebrate from collapsing and impinging upon the nerve roots of the spine. Still further, spinal fusion has been used to restrict motion and stabilize patients' spines by fusing adjacent vertebrate together. This generally can reduce mechanical back pain by preventing the now immobile vertebrate from impinging on a spinal nerve; however, such stability and pain reduction generally is created at the expense of spinal flexibility and motion. In addition, many conventional techniques for disc repair and replacement can be limited in terms of their size or configuration and thus generally are not designed to accommodate variations in size of the gap resulting from the excising of the vertebral disc material. Further, conventional techniques often cannot accommodate expansion or growth of the spine, frequently requiring replacement of the vertebral spacers with other, different size spacers.
Accordingly, it can be seen that a need exists for a vertebral body replacement and system and method of implanting such a vertebral body replacement that addresses the forgoing related and unrelated problems in the art.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A-1C are perspective illustrations of various alternative embodiments of the vertebral body replacement member according to the principles of the present invention.
FIG. 2 is an exploded perspective illustrating the installation of the vertebral body replacement member such as illustrated in FIG. 1A or 1 B within the spinal column of a patient.
FIG. 3 is a perspective illustration, illustrating the distraction of the intervetebral body replacement member according to the principles of the present invention positioned between adjacent vertebrate of the patient's spine to enable insertion of a spacer therebetween.
DESCRIPTION OF THE INVENTION
As generally illustrated in FIGS. 1A-1C , the disclosed apparatus is directed to a vertebral body replacement member or elements for insertion into an intervertebral space or gap between vertebrae of a patient's spine to replace substantially all of a vertebral disc or vertebrae that has been excised or removed due to damage or degeneration of the disc. The vertebral body replacement member generally is useful to replace a vertebral disc that has degenerated due to traumatic injury, vertebral displacement, disease (i.e., autoimmune disease, rheumatoid arthritis, etc.), or any other pathological condition of the spinal column that may injure or shift the intervetebral discs. The vertebral body replacement member provides support to the adjacent vertebrae of the patient's spine to help maintain the separation between the vertebrae, while also preserving the natural curvature of the spine and further enabling regenerative bone growth and adjustment of the intervertebral spacing between the adjacent vertebrae to accommodate growth or expansion therebetween.
It is generally contemplated that the vertebral body replacement member can be made from any bio-compatible or physically inert material or combination of such materials having the mechanical strength capable of maintaining the intervetebral space between adjacent vertebrae, as indicated in FIGS. 2 and 3 , without impinging upon nerves and/or restricting movement and further bone growth or regeneration of the spinal column discs adjacent the intervetebral space in which the disclosed apparatus is mounted. Examples of such materials can include bone, such as bone sections from a femur or other bones of the patient or from donors, metal materials such as titanium, titanium alloys, stainless steel, chrome, cobalt, and other, similar materials, as well as various polymeric materials such as methyl methacrylate (MMA), urethane, polyacetal material, reinforced polymers such as carbon fiber or polyether keytone, polycarbonates, polypropylene, polyamides, and silicone based polymers as generally understood in the art.
As illustrated in FIGS. 1A-1C , the vertebral body replacement member generally includes a telescoping construction, including an upper section and a lower section. Turning now to FIG. 1A , an upper section 12 and a lower section 13 of the vertebral body replacement member 11 engage or interface via a sliding joint which allows relative linear motion in the direction of an axis of linear motion 14 . Assembly, adjustment, and removal of the vertebral body replacement member 11 is enhanced with the sliding joint because the sections advantageously move more freely than with other attachment or interfacing means. While alternate attachment or interfacing means may be available, an acceptable alternate does not include a threaded means. The upper section 12 and the lower section 13 can be formed in various configurations or cross sections. Such configurations generally include a cylindrical configuration, having a substantially circular cross section as illustrated in FIGS. 1A and 2 ; a generally cylindrical configuration with a substantially oval cross-section as illustrated in FIG. 1B ; or in square or rectangular configurations as generally illustrated in FIGS. 1C and 3 . Among other functions, the non-circular embodiments have the added benefit of restricting longitudinal rotation relative to the axis of linear motion 14 between the upper section 12 and the lower section 13 . An alternate means of restricting longitudinal rotation between the upper and lower sections from those disclosed in FIGS. 1B and 1C would be a key and keyway interface (not illustrated). In some applications, restriction of longitudinal rotation is desired and is accomplished by the non-circular alternate embodiments. The circular configuration is advantageous in that although longitudinal rotation is not required, it is possible, while providing relative linear motion of the upper section 12 and the lower section 13 . Further, as illustrated in FIG. 1A , with a top surface 15 and a bottom surface 16 angled or contoured as discussed below, restricting longitudinal rotation of the upper section 12 and the lower section 13 is desired. Each of the upper section 12 and the lower section 13 further generally includes an open-ended body formed from a bio-compatible or physically inert material as discussed above, and one of the sections, for example the upper section 12 , will be formed with at least a portion of its body having a slightly smaller diameter or cross-sectional area than the lower section so as to telescope into and out of the open upper end of the lower section 13 as indicated in FIGS. 1A-1C . It will, however, also be understood that the upper section 12 and the lower section 13 can be formed with the lower section 13 telescoping into and out of the upper section 12 as needed or desired.
The open ended structures of the upper section 12 and the lower section 13 further generally define a space or cavity 17 within the vertebral body replacement member 11 as the two sections 12 , 13 are brought together. The upper section 12 generally includes a substantially flat top surface 15 that further can include channels 17 or openings formed therein, and, as illustrated in FIGS. 1A and 1B , further can include a series of teeth or serrations 19 formed about the side edge 20 of the top surface 19 of the upper section 12 to help secure it against an adjacent upper vertebrae (not illustrated). The lower section 13 typically has a similar construction, with an open upper end, a closed, substantially flat bottom surface 16 , and further generally includes slots 21 or openings formed in its bottom or base plate. The lower section 13 also can include series of teeth or serrations 22 formed about the side 23 of its lower or bottom base plate to help engage and fix the lower section 13 to the lower vertebrae (not illustrated) of the patient's spine in which it is mounted. Additionally, an upper portion of the lower section 13 may also include teeth or serrations 24 , further aiding in support of the component 11 to the vertebrae. The top surface 15 and the bottom surface 16 of the upper section 12 and the lower section 13 , respectively, additionally can be angled or contoured as needed to substantially match the contour of the adjacent upper and lower vertebrae on which the sections 12 , 13 are mounted or engaged.
Openings 25 are formed in top 126 and bottom 27 portions of the upper section 12 and the lower section 13 , respectively, of the vertebral body replacement member 11 and provide areas or points of access for bone to grow and expand into the surrounding tissue about the patient's spine to help further secure the vertebral body replacement member 11 within the patient's spine and to foster or facilitate regeneration and additional bone growth. As illustrated in FIG. 1C , growth openings 42 are also formed in the side walls thereof. The telescoping construction of the vertebral body replacement member 11 further enables the vertebral replacement member 11 to expand or extend as needed to accommodate such additional or regenerative bone growth and to enable further adjustment of the spacing provided by the vertebral body replacement member 11 as needed to fit the intervetebral space created by the excising or removal of part or the entirety of the damaged vertebral disc.
As further illustrated in FIG. 1A , the upper section 12 and the lower section 13 each generally include a large slotted opening 26 formed through the side wall or walls of the upper section 12 and the lower section 13 of the vertebral body replacement member 11 . This opening 26 enables the insertion and packing of bone material within the cavity 17 defined between the upper section 12 and the lower section 13 of the vertebral body replacement 11 member after implantation or placement of the vertebral body replacement member 11 within the patient's spine. Such implanted bone material can then fuse to and grow with the existing remaining vertebrae of the patient, expanding out through the openings 26 formed in the top 15 , bottom 16 , and upper side wall 28 of the upper section 12 and lower side wall 29 of the lower section 13 , respectively, of the vertebral body replacement member 11 and into contact with the adjacent upper and lower vertebrae and the tissue surrounding the patient's spine.
Alternate embodiments of the vertebral body replacement member are illustrated in FIGS. 1B and 1C . FIG. 1B illustrates a vertebral body replacement member 31 having an upper section 32 and a lower section 33 . The upper section 32 and the lower section 33 assemble such that the two sections 32 , 33 fit together in a telescopic fashion. The upper section 32 and the lower section 33 are oval in cross section, thus preventing relative rotation between the two sections 32 , 33 . In this embodiment, the upper section 32 has a lower portion 34 with a reduced diameter from an upper portion 35 . A lip 36 is formed at the interface of the upper portion 35 and the lower portion 34 . When the upper section 32 and the lower section 33 are assembled, the lip 36 rests on, or comes into contact with, a rim 37 of the lower section 33 and establishes a length of the vertebral body replacement member 31 . Illustrated in FIG. 1C , a vertebral body replacement member 41 is shown having an upper section 43 and a lower section 44 with the upper section 43 and lower section 44 being square, or rectangular, in cross section. A spacer 45 fits between the upper section 43 and the lower section 44 and establishes, among other things, a length of the vertebral replacement body member 41 . The spacer 45 may also increase the overall rigidity of the component 11 , help absorb shock during use, reduce component 41 wear, and reduce the amount of packing material necessary. When assembled, the spacer 45 may be contained within a cavity 46 and rest on a base 47 of the lower section 44 .
Still further, as illustrated in FIG. 3 , the upper section 62 and the lower section 63 of the vertebral body replacement member 61 further generally will include a distraction slot 64 or similar opening for receiving a distracter instrument 65 or tool therein. Alignment of the distraction instrument 65 or tool with the distraction slot 64 is preserved because of the restriction of relative longitudinal rotation between the upper section and lower section in the non-circular embodiments (and the circular embodiment with keyways or other restrictive rotational restraints). The ends of the distracter instrument 65 will be introduced into the distraction slots 64 formed in the upper section 62 and the lower section 63 for placement of the vertebral body replacement member 61 within the vertebral space or excised area between the adjacent vertebrae 55 , 56 and thereafter expanding the sections as needed by causing the upper section 62 and the lower section 63 to telescope or move outwardly in a direction of travel 68 away from each other so as to expand the intervertebral body replacement member 61 as needed to fill the intervertebral space.
In addition, as illustrated in FIGS. 2 and 3 , one or more spacers 69 (spacers are seen as 54 in FIG. 2 ) also can be mounted between the upper and lower sections of the vertebral body replacement member as needed. Turning now to FIG. 2 , the spacers 54 generally will be made from the same or a compatible material as the upper section 52 and the lower section 53 of the vertebral body replacement member 51 and typically will be of a similar configuration and/or size as the upper section 52 and the lower section 53 so as to fit therebetween without substantially overlapping the side edges of the upper section 52 and the lower section 53 and, provide a more mechanically robust and rugged structure due to the superior load carrying abilities of a nested structure in compression having a large load bearing surface. For example, as illustrated in FIGS. 2 and 3 , the upper section 52 , 62 of the vertebral body replacement member 51 , 61 can include a bottom portion 57 , 67 formed with a reduced area or diameter that is adapted to be received and telescope into the open upper end 58 , 66 of the lower section 53 , 63 . The spacers 54 , 69 can be of a similar size and configuration as the upper section 52 , 62 and the lower section 53 , 63 so as to fit over this recessed portion 57 , 67 of the upper section 52 , 62 . The spacers 54 , 69 also can be provided with teeth (not shown) as needed to help secure the spacers in place within the intervertebral space, between the adjacent vertebrae 55 , 56 . The spacer 54 , 69 may be configured as a hollow band (for example, but not limited to, a cylindrical ring or rectangular band), having an inner diameter or inside perimeter that is similar to the diameter or perimeter of the recessed portion 57 , 67 . The terms “ring” and “band” are used interchangeably in this disclosure. The ring shaped spacer 54 , 69 may also be a split ring (or split band) to facilitate assembly. As a ring, the spacer 54 , 69 is free to slide telescopically along the recessed portion 57 , 67 so when assembled, the lower surface 59 , 79 of the spacer 54 , 69 will rest against the upper rim 60 , 80 of the lower section 53 , 63 thereby establishing the length of the vertebral body replacement member 51 , 61 .
The spacers 54 , 69 typically will be inserted as needed after implantation of the vertebral body replacement member 51 , 61 within the intervetebral space, by engagement of the upper section 52 , 62 and the lower section 53 , 63 of the vertebral body replacement 51 , 61 member by the distraction tool (see FIG. 3 ) and expansion thereof, so as to create a gap in which the spacer(s) 54 , 69 can be inserted. Thereafter, as the distraction instrument is closed, the upper section 52 , 62 and the lower section 53 , 63 of the vertebral body replacement member 51 , 61 will be brought together, sealing into engagement with each other and with any spacers 54 , 69 contained therebetween. Thereafter, the distraction tool or instrument can be removed and the surgical opening in the patient's back closed. Still further, if additional spacers 54 , 69 are needed, the distraction tool can be engaged with the slots in an upper slot 71 , 64 and a lower slot 72 , 64 and the upper section 52 , 62 and the lower section 53 , 63 further separated to enable implantation of a additional spacers 54 , 69 as needed.
The present invention thus provides a simple device, typically made from a single, biocompatible material with minimal parts and generally utilizing only a minimal presences of screws, if at all, or similar fasteners to attach the upper and lower sections of the vertebral body replacement member to the adjacent vertebrate of the patient. The vertebral body replacement member further is radiolucent and expandable, and any distraction required is done by distracting the device internally through the engagement of the distraction instrument with the slotted openings in the upper and lower sections thereof, such that there is no distraction or engagement of screws that could damage bone. The growth openings formed in the top, bottom and side walls of the upper and lower sections, respectively, further enable bone growth out of the vertebral body replacement member and into the surrounding bone and tissue to help promote healing and more natural freedom of movement, while maintaining the intervetebral space and preventing collapse of the patient's spine.
It will be understood by those skilled in the art that while the foregoing has been described with reference to preferred embodiments and features, various modifications, variations, changes and additions can be made thereto without departing from the spirit and scope of the invention. | This invention concerns a vertebral body replacement element to be inserted into an intervertebral space, thus supporting the spinal column of a patient. The vertebral body replacement element has a hollow upper member and a hollow lower member, with the upper member and lower member engaging in a telescopic manner and establishing a cavity between the two members when assembled. Spacers may be inserted in the cavity to lengthen the vertebral body replacement element. The present invention further concerns a system and method for expanding and distracting a vertebral body replacement element into and within the spinal column of a patient. | 0 |
BACKGROUND
This invention generally relates to power tools and, more particularly, to portable, electrically-powered power tools, such as, for example, for pumping fluids as in a handheld battery-powered grease gun.
A conventional handheld battery-powered grease gun generally comprises a housing including a head portion and a handle portion extending transversely from the head. A cylindrical barrel holding a supply of grease is removably secured to the head and extends from the head alongside the handle. The head portion includes a pump mechanism including a piston that reciprocates in a bore that forms a pump cylinder. The head portion has an inlet port in communication with the bore and the material in the barrel and an outlet port at one end of the bore to a flexible hose for delivering grease to a point of lubrication.
An electric motor is accommodated in the housing and a gear transmission mechanism is provided between the motor and the pumping mechanism for changing the rotating motion of the motor output shaft to the linear reciprocating motion of the piston while reducing the rotational speed and increasing torque. The transmission of these type mechanisms usually ends in a rotary crank plate having an eccentrically located crank pin that is drivingly disposed within a slot of a reciprocating yoke coupled to the piston. This arrangement has been used primarily in jigsaws, which are the most common type of power tool employing a reciprocating drive mechanism. Batteries to power the motor and the switch to control the operation of the power tool are also found in the housing.
In a battery-powered grease gun, the transmission is needed for dispensing grease under pressure. In order for the grease gun to perform satisfactorily, significant force must be exerted. This requirement has led to the development of large, heavy power transmission mechanisms, resulting in awkward and difficult to handle grease guns. The power requirement also reduces the life cycle of the rechargeable battery. Moreover, since the transmission drive system includes numerous components, the manufacturing is relatively complicated and costly.
Another problem that effects all power tools, including a battery-powered grease gun, is heat build-up within the housing during use of the power tool. Heat build-up can shorten the life of the motor and other moving parts, and is particularly a problem when a housing is made of plastic. Thus, care must be taken to ensure good heat dissipation. For this reason, the electric motor used in power tools typically includes a fan for cooling air circulation. Conventionally, the fan is mounted on the motor armature shaft for generating air flow through openings in the motor and the tool housing. Vents in the tool housing facilitate air flow between the interior of the housing and the atmosphere. The need for good cooling air flow around the motor necessitates placing the motor in a position in the housing to allow sufficient air flow around and through the motor. Unfortunately, the motor position necessitates an arrangement that results in an unfavorably located center of gravity which does not facilitate overall handling of the power tool.
Yet another problem that effects all grease guns, whether battery-powered or manual, is blocked, or “frozen”, grease fittings. The frozen fitting will not allow grease from the grease gun to reach a desired point of lubrication. Occasionally, the frozen fitting can be cleared if enough pressure can be generated by the grease gun. However, a conventional battery-powered grease gun generates only from about 2900 psi to about 6000 psi of pressure, which often is not sufficient to overcome the frozen fitting. As a result, the defective fitting is usually removed and cleaned or replaced.
For the foregoing reasons, there is a need for a power transmission which is compact, yet efficient and powerful enough to be used in power tools, such as battery-powered grease gun. There is also a need for improved cooling in power tools so as to allow more convenient placement of the motor. Ideally, the motor could be positioned in the handle to further reduce the size and improve the handling of the power tool. There is also a need for a battery-powered grease gun which generates a high output pressure for potentially overcoming frozen grease fittings.
SUMMARY
According to the present invention, a grease gun is provided for enhancing the pressure applied to a blocked grease fitting. The grease gun comprises a housing including a handle portion and a head portion. The head portion has a bore forming a pump cylinder, and an inlet passage and an outlet passage extending from the exterior of the head portion and opening into the bore. The outlet passage opens into the bore at a point axially spaced in a first direction from the opening of the inlet passage into the bore. A grease supply cylinder is sealingly secured to the head portion so that the bore is in fluid communication with the grease in the supply cylinder. An electric motor is provided as well as a battery for energizing the motor and a circuit interconnecting the battery and the motor. The circuit includes a switch operable by a user for manually activating the motor when the switch is actuated and a thermal protector for breaking the circuit at a predetermined temperature. A transmission is operably connected to the motor. The transmission comprises a planetary gear assembly including an output gear and a drive gear meshing with the output gear. The drive gear includes a drive pin eccentrically mounted on a face of drive gear. The drive pin is received in a cam slot in a yoke for reciprocation of the yoke by the drive pin upon rotation of the drive gear. A piston is fastened to the yoke at one end and the other end of the piston is slidably disposed in the bore for reciprocal movement relative to the housing. The piston is movable between a first position axially spaced in a second direction from the opening of the inlet passage into the bore and a second position past the inlet passage opening in the first direction. The piston moves toward the outlet passage opening in the first direction through a pumping stroke for forcing the grease in the bore out through the outlet passage opening. The piston moves away from the outlet passage and past the inlet passage opening in the second direction through a return stroke for priming the bore. When the switch is continuously actuated, the thermal protector cycles between an open circuit condition and a closed circuit condition when the discharge hose is connected to a blocked grease fitting. The pressure in the bore and discharge hose increase each time the thermal protector resets to the closed circuit condition up to a maximum pressure.
Also according to the present invention, a method is provided for operating the grease gun. The grease gun operating method comprises the steps of providing a thermal protector for breaking the circuit at a predetermined temperature, actuating the switch, maintaining the switch in the actuated position until the thermal protector reaches the predetermined temperature and breaks the circuit, and continuing to maintain the switch in the actuated position until the thermal protector resets for completing the circuit and again energizing the motor. This method causes the pressure in the grease gun to increase with each cycle of the thermal protector.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the present invention, reference should now be had to the embodiments shown in the accompanying drawings and described below. In the drawings:
FIG. 1 is a perspective view of a battery-powered grease gun according to the present invention;
FIG. 2 is an exploded view of the battery-powered grease gun shown in FIG. 1 ;
FIG. 3 is an exploded perspective view of an electric motor and mounting plate for use in the battery-powered grease gun according to the present invention;
FIG. 4 is a perspective view from the other side of the mounting plate shown in FIG. 3 ;
FIG. 5 is a perspective view of an electric motor mounted in the battery-powered grease gun according to the present invention, with surrounding components cut-away;
FIG. 6 is a side elevation fragmentary view of the battery-powered grease gun shown in FIG. 1 with the right handle part removed;
FIG. 7 is a partial cross-section fragmentary view of the battery-powered grease gun shown in FIG. 1 ;
FIG. 8 is an end elevation view of the battery-powered grease gun shown in FIG. 1 with the handle portion of the housing removed;
FIG. 9 is a side elevation view of a left hand handle part for use in the battery-powered grease gun according to the present invention;
FIG. 10 is a cross section of the handle portion of the housing of the battery-powered grease gun shown in FIG. 1 and taken along line 10 — 10 of FIG. 11 ;
FIG. 11 is a side elevation view of the battery-powered grease gun shown in FIG. 1 with the internal components shown in phantom to depict air flow through the housing during operation of the battery-powered grease gun according to the present invention;
FIG. 12 is a perspective view of a thermal protector for use in a battery-powered grease gun according to the present invention; and
FIG. 13 is a side elevation fragmentary view of the thermal protector shown in FIG. 12 mounted in the battery-powered grease gun according to the present invention.
DESCRIPTION
Certain terminology is used herein for convenience only and is not to be taken as a limitation on the invention. For example, words such as “upper,” “lower,” “left,” “right,” “horizontal,” “vertical,” “upward,” and “downward” merely describe the configuration shown in the Figures. Indeed, the components may be oriented in any direction and the terminology, therefore, should be understood as encompassing such variations unless specified otherwise.
Referring now to the drawings, wherein like reference numerals designate corresponding or similar elements throughout the several views, an embodiment of the present invention is shown in the form of a battery-powered grease gun, designated generally at 20. It is understood that, although the present invention will be described in detail herein with reference to the exemplary embodiment of the battery-powered grease gun 20 , the present invention may be applied to, and find utility in, other portable, hand-held power tools. As described above, electric motors are used in a wide variety of applications involving power tools such as, for example, drills, saws, sanding and grinding devices, yard tools such as, for example, edgers and trimmers, and the like. Further, although the present invention will be described in detail herein as embodied in a power tool wherein rotating motion of the electric motor is converted to linear reciprocating motion, it is not intended to be so limited. The present invention may be used in rotary power tools, such as power drills, screw drivers, and the like, and in kitchen appliances such as, for example, mixers and blenders. Thus, the present invention has general applicability to any device powered by an electric motor wherein improvements in efficiency and cooling are desired.
Referring now to FIG. 1 , the grease gun 20 comprises a housing 22 , including a rear handle portion 24 and a front head portion 26 . The housing 22 , as viewed from the side, is generally L-shaped with the handle 24 extending transversely from an upper end of the head 26 . The handle 24 is generally tubular and of a length somewhat greater than the width of a human hand, and of a girth such that the handle 24 may be readily grasped in the hand of the user. The handle 24 may be contoured so that the handle 24 may be grasped comfortably. A rechargeable battery pack 28 is mounted to the housing 22 at the rear end of the handle 24 . A manually operated trigger 30 extends from an opening in the side of the handle 24 . In this position, the trigger 30 can be selectively operated by manual manipulation by the user gripping the handle 24 to control the flow of electric current from the battery pack 28 to an electric motor (not shown in FIG. 1 ) in the housing 22 .
A tubular reservoir 32 is removably secured to the housing 22 at a lower end of the head 26 for holding a supply of grease. The reservoir 32 is aligned substantially parallel with the longitudinal axis of the handle 24 . It is understood that the term “substantially parallel” as used in this context throughout this specification means more parallel than not. A discharge hose 33 extends from the lower end of the head 26 for delivering grease to desired points of lubrication. It is understood that a wide variety of fluids other than grease, or other lubricant, can be dispensed according to the present invention, such as, for example, sealants such as caulk, glue, cake frosting as well as other high viscosity fluids or semi-solid materials that require high pumping pressure to achieve adequate flow rates.
As best seen FIG. 2 , the handle 24 may be formed as two complementary, symmetric parts such that the handle 24 is in effect split in half along a central longitudinal plane forming a right hand handle part 36 and a left hand handle part 38 , as viewed by the user holding the gun in his right hand with the head 26 at the top. The two handle parts 36 , 38 are joined together in a conventional manner using fasteners, such as screws, an adhesive, welding, or a combination thereof. As depicted in the present embodiment, screw holes 40 are formed in the two handle parts 36 , 38 for fastening the handle parts together. The handle 24 may be made of various materials, including plastics or metals. Preferably, the handle 24 is made of an electrically insulating material with low heat conductivity, such as hard plastic.
The head 26 is generally a rectangular shape with rounded corners and parallel side walls extending between and interconnecting irregular front and rear walls. The upper end of the head 26 has a cylindrical pass through opening 42 . The head 26 is preferably a metal casting.
Referring now to FIGS. 2 and 3 , the electric motor 50 includes a substantially cylindrical motor housing 52 having a side wall 54 with an external surface, a front end wall 56 and a rear end wall 58 . The side wall 54 has two diametrically opposed, circumferentially-extending air ports 60 opening at the external surface of the motor housing 52 . The front end wall 56 has four spaced air ports 62 . An axial rotary output shaft 66 extends from the front end wall 56 of the motor housing 52 . A fan (not shown) is located within the motor housing 52 and attached to the motor shaft 66 . Preferably, the fan is an impeller type fan.
A circular mounting plate 70 is provided for securing the motor 50 in the handle 24 . The mounting plate 70 has front surface 72 and a rear surface 74 ( FIG. 4 ). The rear surface 74 of the mounting plate 70 has four circumferentially spaced recesses 76 having a substantially triangular shape. The mounting plate 70 is adapted to be fastened to the front end wall 56 of the motor housing 52 with the motor shaft 66 extending through a central opening 78 in the mounting plate 70 . The mounting plate 70 is positioned relative to the motor housing 52 such that the apertures 76 in the rear surface 74 of the mounting plate 70 are aligned with the air ports 62 in the front end wall 56 of the motor housing 52 . The mounting plate 70 is fastened to the motor housing 52 using screws 80 which pass through holes 82 in the mounting plate 70 and are received in threaded openings 84 in the front end wall 56 . The motor housing 52 with attached mounting plate 70 is aligned with the opening 42 in the upper end of the head 26 , as best seen in FIGS. 5 and 6 . The mounting plate 70 is fastened to the head 26 using screws 86 which pass through openings in ears 88 circumferentially spaced on the periphery of the mounting plate 70 and are received in threaded openings in the head 26 . The mounting plate 70 is large enough to cover the opening in the head portion. A washer 89 ( FIG. 2 ) is positioned between the mounting plate 70 and head 26 . As seen in FIG. 5 , the rear end wall 58 of the motor housing 52 has four spaced air ports 64 . When the motor 50 is operating, the fan rotates to draw air through the air ports 62 , 64 in the front and rear end walls 56 , 58 of the motor housing 52 to cool the motor 50 . Warmed air is exhausted from the motor housing 52 through the side wall air ports 60 . A suitable motor for use in a power tool according to the present invention is available from Johnson Electric Engineering Ltd. of Hong Kong, and sold as model number HC683LG.
The motor 50 drives a transmission that drives a pump assembly for pumping grease under pressure from the reservoir 32 through the discharge hose 33 . In one embodiment of the present invention, the transmission comprises a planetary gear reduction system, preferably a two-stage planetary gear reduction system housed in the opening 42 in the upper end of the head 26 , which serves as a gear housing. Referring to FIGS. 2 and 7 , a first planetary gear set of the planetary gear system includes three planet gears 96 (only one of which is shown in FIG. 2 ) rotatably mounted on pins 98 extending from a rear surface 99 of a first carrier 100 . A pinion gear 102 is press fit onto the distal end of the motor shaft 66 and forms a part of the transmission. The pinion gear 102 fits between and meshes with the three planet gears 96 on the first carrier 100 . The three planet gears 96 also mesh with an orbit gear 104 fixed in the opening 42 in the head 26 . The orbit gear 104 has four longitudinal ridges 106 ( FIG. 2 ) circumferentially spaced about the periphery. The head 26 has corresponding longitudinal slots 108 formed in the wall defining the upper opening 42 for non-rotatably receiving the orbit gear 102 .
A sun gear 110 is axially mounted to a front surface of the first carrier 100 for rotation with the first carrier. The sun gear 110 meshes with and drives three planet gears 114 (only one of which is shown in FIG. 2 ) of a secondary planetary gear set of the transmission. The second set of planet gears 114 are rotatably mounted on pins 116 extending from a rear surface 118 of a second carrier 120 and also mesh with the orbit gear 104 . An axial reduced diameter shoulder 122 extends forwardly from a front surface of the second carrier 120 . A roller bearing 126 is positioned between the cylindrical peripheral surface of the shoulder 122 and the interior surface of the head 26 . An output gear 128 is fixed to the second carrier 120 at a front surface of the shoulder 122 for rotation with the second carrier 120 . An axial shaft 130 extends from the spur gear 128 and is received in a bore in a semi-circular bracket 132 fastened to the front wall of the head 26 . The shaft 130 is supported for rotation in the bracket 132 by a needle bearing 134 .
A drive gear 140 is provided at the forward end of the transmission. An axial shaft 146 extends from a rear surface 144 of the drive gear 140 and is rotatably received in a pass through axial bore 148 in the head 26 below the upper opening 42 . The axial shaft 146 is supported in the bore 148 by a needle bearing 150 and a ball bearing 151 positioned between two retaining clips 153 . The front clip 153 fits in a groove in the interior surface of the bore 148 for maintaining the ball bearing 151 in the bore 148 . The rear clip 153 fits in a groove in the shaft 146 for maintaining the axial position of the shaft 146 . An eccentrically mounted shaft 152 extends transversely from the front surface of the drive gear 140 . A hollow cylindrical drive pin 154 is mounted for rotation on the eccentric shaft 152 between two washers 155 . A retaining clip 156 fits into a groove 157 in the end of the shaft 152 to hold the drive pin 154 in place.
As shown in FIGS. 7 and 8 , a yoke 160 is positioned adjacent to the front surface of the drive gear 140 . The yoke 160 is substantially heart-shaped. A curved oblong cam slot 166 is formed in the yoke 160 . The cam slot 166 is dimensioned to receive the drive pin 154 , allowing sufficient room to enable the drive pin 154 to slide freely through the cam slot 166 from end to end. As depicted in the Figures, a scotch yoke design having a track configuration that minimizes the side load forces imposed on the yoke 160 is preferred. However, it is understood that the configuration of the cam slot 166 may be straight, with the length of the slot 166 equal to the diameter of the circle traced by the drive 154 pin.
Referring again to FIG. 7 , the pump assembly comprises a pump chamber 168 including the lower end of the head 26 . The pump chamber 168 defines a cylindrical bore 170 which, as will be described below, is in fluid communication with the reservoir 32 of grease and the discharge hose 33 . The pump chamber bore 170 receives a plunger 172 in sliding engagement with the interior surface of the bore 170 . The plunger 172 extends upwardly through an opening in the pump chamber 168 . The distal end of the plunger 172 is received in an opening in the yoke 160 and secured in place with a pin 174 . A resilient seal 176 is positioned in an annular recess in the opening in the pump chamber 168 and surrounds the plunger 172 for sealing the pump chamber 168 .
The pump chamber 168 has a circular threaded flange 178 that is internally threaded for receiving an externally threaded open end of the reservoir 32 . A gasket 179 is seated between the head 26 and the reservoir 32 for sealing the connection. The operation of the grease reservoir 32 may be typical of a conventional grease gun that is either manually or battery-powered. Therefore the interior of the reservoir 32 is not shown in the drawings. The grease supply in the reservoir 32 is in fluid communication with the bore 170 via an inlet passage 180 formed in the pump chamber 168 and extending from the recess 178 and opening into the bore 170 . An outlet passage 182 is spaced downward from the inlet passage 180 and extends from the bore 170 to a fitting 184 to which the discharge hose 33 is connected. A ball check valve assembly 186 is positioned in the pump chamber 168 at the end of the bore 170 , and is held in place by a threaded plug 188 .
As shown in FIGS. 2 and 7 , the handle 24 has an opening 190 to accommodate the trigger 30 . The trigger 30 has transverse arms 192 that rotatably fit into opposed bosses 194 in the handle 24 so that the trigger 30 will pivot relative to the handle 24 . A paddle 200 extends forwardly from one of the trigger arms 192 . An electrical switch 196 is mounted in the handle 24 adjacent to the trigger 30 . A torsion spring 198 is mounted around one of the trigger arms 192 . One end of the spring 198 engages the trigger 30 and the other end of the spring engages the interior of the handle 24 for biasing the trigger 30 outwardly of the handle and away from the switch 196 in an “off” position. Two wires carry power from the battery pack 28 to the motor 50 . When the trigger 30 is actuated by the user, the trigger 30 pivots inwardly against the biasing action of the spring 198 . The paddle 200 contacts the switch 196 for moving the switch to an “on” position. When the user releases the trigger 30 , the spring 198 operates to pivot the trigger 30 back to the off position.
In use, the user grips the handle 24 and manually manipulates the trigger 30 to energize the motor 50 , rotating the motor shaft 66 and pinion gear 102 . Rotation of the pinion gear 102 is transmitted through the transmission causing the drive gear 140 to rotate at a reduced speed of rotation and at an increased torque from that of the pinion gear 102 . The rotation of the drive gear 140 is transmitted to the yoke 160 by the action of the drive pin 154 engaging the inside peripheral surface of the cam slot 166 for reciprocating the yoke 160 and plunger 172 .
The plunger 172 reciprocates in the bore 170 of the pump chamber 168 through a pressure stroke and a return stroke. On the pressure stroke, the plunger 172 moves in the bore 170 in a downward direction, as seen in FIG. 7 , past the inlet passage 180 and toward the outlet passage 182 . Grease in the bore 170 is thus pushed toward the outlet passage 182 . Pressure on the grease increases until the ball check valve 186 is unseated and grease under pressure passes through the outlet passage 182 and is discharged through the hose 33 . Once the pressure stroke has been completed, the plunger 172 is retracted upward, as seen in FIG. 7 , away from the outlet passage 182 and back across the inlet passage 180 thereby allowing more grease to enter into the bore 170 .
As best seen in FIGS. 7 and 8 , the bracket 132 partially closes the opening in the upper end of the head 26 . This maintains the axial relationship of the components of the transmission and resists any tendency of the drive gear 140 to tilt or skew relative to its central axis due to forces exerted by the yoke 160 against the drive pin 154 during rotation of the drive gear 140 . As described above, it is understood that other power tools may use this transmission arrangement, including tools with rotating drives wherein rotary movement may continue through to a chuck which is adapted to drive a suitable bit or implement that comes into engagement with the work.
In another embodiment of a battery-powered grease gun according to the present invention, a thermal protector is used to enhance the pressure generated by the grease gun 20 . A thermal protector for this purpose is shown in FIG. 12 and generally designated at 250 . The thermal protector 250 includes two terminals 252 at one end for electrically connecting the thermal protector 250 to wire leads. Referring to FIG. 13 , the thermal protector 250 is shown in position in the left hand handle part 38 of the handle 24 upstream of the motor 50 in the chamber 220 formed in the rear portion of the handle 24 . The thermal protector 250 is electrically connected between the contact assembly 208 and the motor 50 to control the flow of electric current from the battery pack 28 to the motor 50 . Specifically, one of the wires carrying power from the contact assembly 208 to the battery pack 28 leads through the thermal protector 250 to the motor 50 . The other wire leads from the contact assembly 208 to the switch 196 and from the switch 196 to the motor 50 .
The operation of the battery-powered grease gun 20 according to this embodiment is, as described above, by manual manipulation of the trigger 30 for moving the switch 196 to an “on” position to energize the motor 50 . The motor 50 causes rotation of the drive gear 140 which rotation is transmitted to the yoke 160 by the action of the drive pin 154 engaging the inside peripheral surface of the cam slot 162 in the yoke 160 . The yoke 160 is connected to the plunger 172 which reciprocates in the bore 170 forcing grease under pressure through the outlet passage 182 . The grease is discharged through the hose 33 to a desired point of lubrication. However, if the discharge hose 33 is connected to a blocked grease fitting (not shown), grease will not flow, causing pressure to build in the bore 170 and the discharge hose 33 . Because the electric motor 50 has to work against the pressure, the current passing through the thermal protector 250 increases, thereby increasing the temperature of the thermal protector 250 . Eventually, the thermal protector 250 reaches a pre-calibrated temperature at which point the thermal protector 250 functions to open the circuit. It is understood that this temperature is reached during a fault condition caused by an increase in electric current flowing through the thermal protector 250 and not an increase in the ambient temperature. In the present configuration of the grease gun 20 described herein, the thermal protector 250 opens the circuit shortly after the pressure in the grease gun 20 reaches about 7000 psi.
After the thermal protector 250 breaks the circuit, the motor 50 stops and the thermal protector 250 cools. When the temperature of the thermal protector 250 is again below the pre-calibrated temperature, the thermal protector 250 will automatically reset. Because the ambient temperature is below the pre-calibrated temperature, the thermal protector 250 cools quickly and will reset within several seconds. If the user continues to actuate the trigger 30 for maintaining the switch 196 in the on position, power will again be delivered through the circuit for energizing the motor 50 . If the grease fitting remains blocked, the current increases rapidly and the thermal protector 250 again opens the circuit. The thermal protector 250 will cool quickly and reset, and this cycle will repeat indefinitely. Importantly, each time the circuit cycles between the open condition and the closed condition, the pressure in the bore 170 and the discharge hose 33 of the grease gun 20 increases. As the thermal protector 250 continues to cycle, the pressure will continue to increase up to about 10,000 psi, after which there will be no further increase in pressure even if the thermal protector 250 continues to cycle. Moreover, it is understood that the high pressure generated by the cycling of thermal protector 250 increases the likelihood of clearing the blocked grease fitting.
It has been observed that when the thermal protector 250 opens the circuit, the high pressure in the bore 170 causes the plunger 172 to move upwardly in the bore 170 from a position where the plunger 172 has stalled, which always occurs during the pressure stroke. Since this is opposite to the direction of movement of the plunger during the pressure stroke when the grease gun 20 is powered, upward movement of the plunger 172 back drives the drive gear 140 , transmission and electric motor 50 by the action of the drive pin 154 in the cam slot 162 of the yoke 160 . As the plunger 172 retreats, additional grease is drawn into the bore 170 through the inlet passage 180 . When the thermal protector 250 resets, the plunger 172 is driven downward in the bore 170 , although the plunger 172 may or may not reach the previous stall position.
A suitable thermal protector for use in the battery-powered grease gun according to the present invention is available from Texas Instruments and sold under device code 7AM029A5-YYY. This thermal protector is pre-calibrated to open the circuit at a temperature of 110° C.+/−5° C. However, as described above, when the grease gun 20 is used with a blocked grease fitting, the fault condition of the thermal protector 250 is typically reached due to an increase in current rather than as a result of the ambient temperature reaching the pre-calibrated temperature. Thus, the cycling of the thermal protector 250 for building pressure in the grease gun 20 may be achieved using thermal protectors having a broad range of pre-calibrated opening temperatures. Preferably, the thermal protector 250 is selected to have a pre-calibrated opening temperature that is not reached during normal operation of the grease gun 20 in the absence of a blocked grease fitting.
FIG. 9 shows the interior of the left hand handle part 38 . It is understood that the interior of the right hand handle part 36 is a mirror image of the left hand handle part 38 . The left hand handle part 38 includes inwardly projecting integral walls. An upper battery socket wall 202 and a lower battery socket wall 204 are formed at the rear end of the handle parts 38 and are configured to accommodate the battery pack 28 . The inner ends of the battery socket walls 202 , 204 have transverse slots 206 for receiving a contact assembly 208 for connection to the battery pack 28 . A partition wall 210 extends radially inward in the handle 24 forward of the battery socket walls 202 , 204 . The partition wall 210 has a central semi-circular cutout 212 . The internal walls of the handle 24 provide strength and rigidity to the handle 24 .
When the handle parts 36 , 38 are assembled, the entire length of the battery socket walls 202 , 204 and the straight lengths 214 of the partition walls 210 contact one another. The semi-circular cutouts 212 of the partition wall 210 define a central opening in the handle 24 which surrounds and seals against the periphery of the side wall 54 of the motor housing 52 . As best seen in FIGS. 7 and 10 , the partition walls 210 seal against the motor housing 54 adjacent to and rearward of the air ports 60 in the side wall 54 . A slot 216 is formed in the partition wall 210 for allowing the wires 199 from the contact assembly 208 to pass. The slot 216 is sized to minimize clearance between the wires 218 and the partition 210 ( FIG. 9 ).
The partition wall 210 divides the interior of the handle 24 into two separate chambers when the handle parts 36 , 38 are joined. Specifically, a chamber 220 is formed in the rear portion of the handle 24 upstream of the motor 50 . The upstream chamber 220 is defined by the interior surface of the rear portion of the handle 24 , the partition wall 210 and the upper and lower battery socket walls 202 , 204 . Forward of the partition wall 210 is an exhaust air chamber 222 defined by the interior surface of the forward portion of the handle 24 , the partition wall 210 and the exterior surface of the head 26 . Air vents 224 , 226 are formed in the front portion and rear portion of the handle 24 . The exhaust chamber 222 and the upstream chamber 220 are in communication with the atmosphere via the vents 224 , 226 in the front and rear portions of the handle, respectively.
Air flow through the housing 22 is generated by rotation of the fan on the motor shaft 66 when the motor is running. Referring to FIGS. 1 , 5 , 6 and 11 , dotted lines with arrows in the Figures show the direction of air flow through the housing 22 . The motor fan draws ambient air from outside of the housing 22 through the inlet air vents 226 in the rear portion of the handle 24 . Air flows forwardly into the inlet ports 64 in the rear end wall 58 of the motor housing 52 . The partition wall 210 directs substantially all of the air drawn into the rear portion of the handle 24 into the motor housing 52 for cooling the motor 50 . As described above, air flows through the motor 50 and is discharged from the ports 60 in the side wall 54 into the exhaust chamber 222 .
A portion of the warmed air exiting the motor housing 52 through the exhaust ports 60 flows along the outer surface of the motor housing 52 , into the ports 62 in the front end wall 56 and again through the motor housing 52 to be discharged from the side wall ports 60 . The remainder of the exhausted air flows lengthwise of the handle 24 cooling the exhaust chamber 222 of the handle 24 and head 26 prior to exiting the housing 22 through the outlet vents 224 to the ambient. The periphery of the motor housing 52 and mounting plate 70 do not extend to the interior surface of the handle 24 for defining an annular space between the periphery of the motor housing 52 and mounting plate 70 and the interior surface of the handle 24 for the passage of air. The partition wall 210 substantially prevents the re-circulated exhaust air from returning to the upstream chamber 220 in the rear portion of the handle 24 . Where the cross-sectional area of the mounting plate 70 is greater than the cross-sectional area of the motor housing 52 , as in the embodiment of the present invention shown in the Figures, the mounting plate 70 may function to deflect a portion of the motor exhaust air radially of the motor housing 52 ( FIG. 6 ). The recesses 76 in the mounting plate 70 induce a portion of the deflected air to flow into the ports 62 in the front end wall 56 .
It is understood that the structure of the interior of the handle 24 generally confines the air flow through the housing 22 to the path described. The channeled air flow acts to cool the motor 50 to a sufficiently low temperature to prevent excessive heat buildup in the motor housing 52 and handle 24 , which would otherwise be detrimental to either the motor 50 or the housing 22 , particularly a plastic housing, and cause discomfort to the user. This extends the life of the tool components. Moreover, this arrangement allows the placement of the motor 50 in the handle 24 of the grease gun 20 . Placing the motor 50 , battery pack 28 , and transmission in the handle provides a compact, balanced design for any power tool. In a grease gun, wherein the handle 24 is oppositely positioned relative to the grease reservoir 32 , a weight distribution is now available that enables the grease gun 20 to be more easily manipulated while gripping the handle 24 .
Although the present invention has been shown and described in considerable detail with respect to only a few exemplary embodiments thereof, it should be understood by those skilled in the art that we do not intend to limit the invention to the embodiments since various modifications, omissions and additions may be made to the disclosed embodiments without materially departing from the novel teachings and advantages of the invention, particularly in light of the foregoing teachings. For example, any number of planetary gear stages could be used in the transmission depending on the motor construction. Further, the handle construction channeling air flow can be used in a power tool that does not use a planetary gear system in the transmission. Accordingly, we intend to cover all such modifications, omission, additions and equivalents as may be included within the spirit and scope of the invention as defined by the following claims. In the claims, means-plus-function clauses are intended to cover the structures described herein as performing the recited function and not only structural equivalents but also equivalent structures. Thus, although a nail and a screw may not be structural equivalents in that a nail employs a cylindrical surface to secure wooden parts together, whereas a screw employs a helical surface, in the environment of fastening wooden parts, a nail and a crew may be equivalent structures. | A battery-powered grease gun is provided for enhancing the pressure applied to a blocked grease fitting. The grease comprises a circuit interconnecting the battery and an electric motor. The circuit includes a switch operable by a user and a thermal protector for breaking the circuit at a predetermined temperature. When applying grease to a blocked grease fitting, actuating the switch until the thermal protector reaches the predetermined temperature breaks the circuit until the motor cools and the thermal protector resets for completing the circuit and again energizing the motor. Continuing to maintain the switch in the actuated position until the thermal protector resets causes the pressure in the grease gun to increase with each cycle of the thermal protector. | 5 |
CROSS-REFERENCE TO RELATED APPLICATIONS
The present application is a National stage application of PCT/EP03/06864, filed Jun. 27, 2003.
1. Field of the Invention
The present invention relates to a vacuum insulated refrigerator cabinet comprising an evacuation system for evacuating an insulation space of the cabinet when pressure inside such space is higher than a predetermined value.
With the term “refrigerator” we mean every kind of domestic appliance in which the inside temperature is lower than room temperature, i.e. domestic refrigerators, vertical freezers, chest freezer or the like.
2. Discussion of the Prior Art
A vacuum insulated cabinet (VIC) for refrigeration can be made by building a refrigeration cabinet that has a hermetically sealed insulation space and filling that space with a porous material in order to support the walls against atmospheric pressure upon evacuation of the insulation space. A pump system may be needed to intermittently re-evacuate this insulation space due to the intrusion of air and water vapour by permeation. A solution of providing a refrigerator with a vacuum pump running almost continuously is shown in EP-A-587546, and it does increase too much the overall energy consumption of the refrigerator. It is advantageous for energy consumption to re-evacuate only when actually needed. Therefore there is in the art the need of a simple and inexpensive insulation measurement system that would be applicable to operate a refrigerator cabinet vacuum pump or similar evacuation system only when actually needed.
The present invention provides a vacuum insulated refrigerator cabinet having such insulation measurement system, according to the appended claims.
According to the invention the measurement system is a system that measures the insulating value of the VIC insulation. A non-equilibrium measuring approach is taken that requires only one temperature sensor. This sensor is buried in the evacuated insulation material, preferably in a central position thereof with reference to the thickness of the insulation space. At a central position within the insulation space, the disturbances from transients in external surface temperature are minimised. However, the sensor device may be placed in any portion of the vacuum space, but with likely complications due to the transients in external surface temperature. It is also possible to place the sensor device on an external portion of evacuated insulation that is connected by a conduit to the main vacuum insulation chamber, mainly in order to facilitate the mounting of the sensor device. In immediate proximity to the sensor is a heat source that can be pulsed. The thermal pulse is controlled to a small, precise amount of thermal energy. The insulation and the temperature sensor, in the immediate area of the thermal pulse, will show a temporary increase in temperature. The effective thermal conductivity, heat capacity and density of the surroundings of the thermal pulse control the decay of the increase in temperature. Heat capacity and density are expected to remain constant over the life of the refrigerator, but the thermal conductivity will increase due to the deterioration of vacuum level in the insulation. An analysis of the decay will produce a measure of thermal conductivity and allow a criterion for pumping to be applied. Due to the fact that this device is centrally located in the insulation, relieves the problems of outside temperature variations. At any rate it is possible to apply the device to the external wall of the insulation space and protect it with an insulating pad. After calibration, this device may just have to record one temperature at a specified time after the application of the temperature pulse for use as the pumping criterion.
BRIEF DESCRIPTION OF THE DRAWINGS
The invention will now be explained in greater detail with reference to drawings, which show:
FIG. 1 is a schematic cross-view of a wall of a vacuum insulated cabinet according to the invention; and
FIG. 2 is a schematic diagram showing the relationship between the temperature measured in the proximity of the heat source and the time, in two different conditions of thermal conductivity.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to the figures, a refrigerator cabinet comprises an insulated double wall 10 comprising two relatively gas impervious walls 10 a (liner) and 10 b (wrapper) filled with an evacuated porous insulation material 12 . Both liner 10 a and wrapper 10 b may be of polymeric material. The insulation material 12 can be an inorganic powder such as silica and alumina, inorganic and organic fibers, an injection foamed object of open-cell or semi-open-cell structure such as polyurethane foam, or a open celled polystyrene foam that is extruded as a board and assembled into the cabinet. The insulation material 12 is connected to a known evacuation system (not shown) that can be a physical adsorption stage (or more stages in series) or a mechanical vacuum pump or a combination thereof.
According to the invention, inside the insulation material 12 of the double wall 10 it is buried a temperature probe 14 connected to a control unit 16 . In the proximity of the temperature probe 14 , at a close distance therefrom, it is buried an electric heater 18 also connected to the control unit 16 . The control unit 16 is linked to the system (not shown) for evacuating the insulation material 12 .
According to a second embodiment of the invention, it is possible to use a heated wire as the thermal source and then measure the temperature decay in the wire by using the same wire as a resistance thermometer. In order to assess the performances of the insulation material, the control unit 16 switches on the electric heater 18 for a short period, typically of 1-10 s, and with switching interval preferably comprised between 1 and 30 days. At the same time, the temperature probe 14 measures the sudden increase of temperature around the heater 18 , and the following decay when the heater is switched off. The heater is switched on and off according to a predetermined pulse pattern, whose time interval between pulses may vary broadly according to the insulation material 12 , its width, the material of the liner 10 a and wrapper 10 b and thickness thereof. The decay of temperature ( FIG. 2 ) is highly influenced by the pressure inside the VIC insulation, and therefore by actual thermal conductivity of insulation material 12 . In the left portion of FIG. 2 it is shown an example of temperature decay when the thermal conductivity λ is low (low pressure), while in the right portion of FIG. 2 it is shown an example of temperature decay when the thermal conductivity λ has increased due to an increase of pressure inside the material 12 , for instance after some days from the last intervention of the vacuum pump. If at a predetermined time K the temperature is lower than a threshold value T, then it is time for the control unit 16 to switch on the vacuum pump in order to re-establish the correct performances of the refrigerator. Of course the control unit 16 may also assess when for a predetermined temperature, the time for reaching such temperature is shorter than a threshold value. From the above description it is clear that it is not necessary to detect how the temperature measured by the sensor 14 changes with time, since it is needed to record one temperature only at a predetermined time after the temperature pulse.
The general energy conservation equation for the heat diffusion through a solid medium, in the case of the sensor system according to the present invention, can be approximated as one-dimensional due to the geometric characteristic of domestic refrigerator walls, where one of the dimensions (thickness) is usually much smaller then the other two (height and width). Also, although the thermal conductivity k varies with time, it is not a function of position (spatially invariable), that reduces the equation for heat diffusion to:
K × ⅆ 2 T ⅆ x 2 + q '' = p × c × ⅆ T ⅆ t ( 1 ) k × ∂ 2 T ∂ x 2 + q '' = ρ × c × ∂ T ∂ t ( 1 )
where T is the temperature,
t is time, x is the distance measured across the vacuum wall thickness, k is the thermal conductivity, q″ is the energy generated inside the wall, p is density, and c is the specific heat of the vacuum insulation.
The equation (1) may have several different solutions, depending on the boundary and initial conditions attributed to the dependent variable T, the expression for q″, etc.,
In general, the form of these solutions can be very complex, and for some cases we have to rely on numerical techniques in order to seek the solution for the temperature variation along the time. From computational simulation of the temperature evolution as a function of time it is immediately evident that the largest the thermal conductivity “k”, the steepest the temperature decay.
Due to being located preferably in the centre of the refrigerator insulated wall and because of the thermal capacitance of the vacuum insulation transient, short term changes in the surrounding conditions will be smoothed out and won't affect the “temperature versus time” measured by the temperature probe.
Due to this, the measuring device is practically insensitive to:
door opening, internal temperature switching due to compressor cycling.
Both external (ambient variations) as internal temperature changes (different thermostat set-up) may produce small changes in the probe reading, at some pre-determined time after the pulse heater is switched on. Therefore it is preferred to keep track of internal and external temperatures and feed this information into the logic to control the vacuum pump switching on/off, along with the built-in probe reading.
In view of the above, it is preferred to use thermistors for temperature measurement with accuracy better than 0.2° C. Moreover, it is also preferred to keep track of ambient and internal temperatures, and this information used to “calibrate” the temperature measured according to the present invention. | A vacuum insulated refrigerator cabinet comprises an evacuation system for evacuating an insulation space of the cabinet when pressure inside such space is higher than a predetermined value. The cabinet presents sensor means comprising a temperature sensor and a heater both located within the insulation space and a control system for activating the heater according to a predetermined heating cycle and for receiving a signal from the temperature sensor, such control system being able to provide the evacuation system with a signal related to the insulation level within the insulation space. | 8 |
The invention relates to the arrangement of an impact-sensitive device inside a housing, in particular a transmitter for locating a drill device moving inside a borehole in the ground.
Such drilling devices are known, for example, from the German Offenlegungsschrift 39 00 122 and the European Offenlegungsschrift 0 361 805. Their transmitters have, as a rule, an inclination sensor, a temperature detector, a rotation error sensor, a transmitting antenna and batteries or rechargeable storage batteries. These elements are arranged inside a probe housing with a cover made of a synthetic material or steel which is rigidly attached in an axial bore of the housing of the drilling device.
While the ground drilling takes place, the drilling device can be tracked above the ground due to the signals sent by the transmitter by means of a hand-held receiver or several stationary receivers. To ensure that the transmitter can transmit through the walls of the housing of the device across greater distances, the housing is provided with, for example, four transmission slits 1 to 5 mm wide which are distributed along the circumference and which are closed by means of a synthetic filling material.
The advance of such drilling devices is either through rotary action and/or impact with the result that the drilling device and the transmitter arranged therein are subjected to high dynamic loads. At this time, the transmitter is influenced by, on the one hand, an axial acceleration force due to the rammer and rapid translatory motion, particularly against hard resistances, and, on the other, a radial accelerating force which is created when the drill becomes lodged in stone, or when the drill pipe driving the drilling device by rotation receive a torsional prestress due to the rotary drive when the drill head is suddenly released or, possibly, again becomes lodged.
Such strong accelerating forces result in damage to the transmitter or its components and particularly also to the power supply after a short period of use. Since, as a rule, batteries are used for the power supply of the transmitter, they slam against each other and against the housing due to the high axial accelerating forces, the battery poles become displaced, the batteries are damaged, and the contact interrupted.
Since the failure of the transmitter occurs mostly in deep and hard layers of soil where the highest dynamic loads are found, this means that the drilling device or also the entire drill pipe must be pulled back with the drilling device and disassembled. The transmitter must then be exchanged and the drilling operation restarted. This process becomes particularly lengthy when the device does not hit the old drilling channel, possibly still existing at least in part, but a completely new borehole must be created.
When the drilling device is advanced within the borehole in the soil with the aid of drilling fluid, directed via the drill pipe up to the drilling device, it is important to keep this drilling fluid away from the transmitter. It is possible for the drilling fluid to penetrate into the interior of the housing via a joint between the steering head, mounted on the housing in replaceable fashion, and the housing, as well as through the transmitter slits, when the synthetic sealing material has become detached from the slit wall and falls out. This may result in increased impact transfer to the transmitter and a failure on the part of the transmitter due to the penetration of liquid.
SUMMARY OF THE INVENTION
It is the task of the invention to create an arrangement by means of which impacts and possibly drilling fluid are kept away from the impact-sensitive device in the housing, in particular the transmitter for locating a drilling device moving inside a borehole inside the earth.
Based on this task, in an arrangement of the initially mentioned type, it is proposed that the impact-sensitive device be kept, by means of at least one impact-damping buffer, at a distance from the wall of the chamber accommodating the device, at least in the main direction of impact. The impact-sensitive device may be embedded in the impact-damping buffer or, when it involves a cylindrical transmitter, the impact-sensitive device may be kept at a distance from the wall by means of a buffer arranged at each end.
As a buffer material, preferably silicone rubber with a Shore A hardness of 15 to 30 is used, which has excellent oscillation- and impact-damping properties, which change little across a broad temperature range. Also, the good electrical insulating ability is advantageous.
The impact-damping effect of the buffers in the axial and radial direction is advantageously of such a nature that at least one buffer has a greater diameter than the device and the other buffer has annular grooves.
The annular grooves influence the axial elasticity and deformability of the buffers during axial as well as radial acceleration.
When the buffer is attached in the device by means of at least one pin gripping into a borehole inside the buffer and by means of a snap connection formed between the buffer and the device, where a head on the pin grips into an undercut of the borehole, it is possible for the buffer to be easily connected to or disconnected from the device due to its deformability in order, for example, to service the device. In order to pull the device out of the housing, a pulling hook merely needs to be guided into the undercut in order to then grip the device at the buffer and to be able to pull it out.
In order to enable the device to send a signal that indicates a rotation error to the ground surface, the device must be arranged in the housing without rotational play. For this purpose, at least one of the buffers is connected to the device without rotational play and has an external longitudinal groove, into which a projection on the housing accommodating the device grips to secure against turning. At the other end of the device, a slit, accessible through the borehole of the other buffer, may be arranged for the purpose of positioning tools, for example, a screwdriver.
The connection to the housing without rotational play may also be achieved in that the device is connected to a steering head without rotational play via a torsionally elastic guide rod, which steering head itself is coupled to the housing without rotational play, wherein the guide rod, at its one end, grips via a tab into a front groove at the steering head and is secured, against its being pulled out due to its cross section, while the guide rod, at its other end, grips into a T-groove at the device with a T-tongue. In this way, the complete transmitter can be pulled out of the housing by means of the steering head and, for that purpose, neither a pulling hook nor a screwdriver is necessary for the alignment of the transmitter.
When the T-tongue inside the T-groove exhibits axial play which is greater than the maximally resulting range of elasticity of the buffer and the guide rod is arranged with play inside the borehole of the buffer, the device can oscillate freely without sustaining harmful impact.
Since a drilling device driven by drill pipes is relatively long, it is possible for the drilling device to bend during steering movements, particularly in the presence of very hard soil formations. In order to prevent the cylindrical housing of the impact-sensitive device from coming into contact with the wall of the chamber inside the housing and from becoming stuck, it is advantageous to arrange on the device adjacent to the buffers impact-damping guide rings which may be relatively narrow and have a diameter which is greater than the device by up to 5 mm. In this way, the device can be prevented from becoming stuck during the bending of the drilling device, so that the radial acceleration forces cannot be transferred to the device.
The batteries or rechargeable storage batteries serving as the power supply have a relatively great mass and contact problems between the batteries and the device (transmitter) when particularly high axial accelerations occur. In order to prevent this, it is possible to arrange impact-damping buffers on both sides of a battery arranged in a battery compartment inside the device. If two batteries are arranged coaxially in the battery compartment, the impact-sensitive buffers are arranged preferably on both sides of the batteries, as well as between the batteries and have an annular form so that the battery contacts and/or contact springs can grip through them.
In order to prevent the synthetic filling material that is arranged in the transmitter slits from being separated during the bending of the housing of the drilling device, the transmitter slits may be reinforced by means of crosspieces.
A penetration of drilling fluid from a steering head, attached at the housing, into the device (transmitter), arranged in the housing, can be prevented when at the steering head a lip seal is present, providing a seal with respect to the housing.
BRIEF DESCRIPTION OF THE DRAWING
The invention is explained in greater detail in the following text by means of an example shown in the drawing. In the drawing,
FIG. 1 shows a drilling device with a transmitter arranged therein in an axial, longitudinal section and
FIG. 2 shows the enlarged representation of a cylindrical transmitter with buffers arranged at the ends, in partial cross section,
FIG. 3 shows a detail of the connection between a drill head at the drilling device and the transmitter.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The drilling device (1) consists of a housing (2) whose rear end (3) is provided with threads for the attachment of drill pipes (not shown). By means of a central borehole (4) in the rear end (3) and an eccentric borehole (5) in the housing (2), drilling fluid is directed to a steering head (9), arranged at the head end of the drilling device (1).
A cylindrical chamber (6) for a transmitter (14) is located in the housing (2). In the area of the chamber (6), transmission slits (7) are arranged so that the transmitter (14) can transmit through the drilling device wall across greater distances.
These transmission slits (7) are approximately 1 to 5 mm wide, extend axially essentially across the length of the transmitter (14) and are reinforced with one or several crosspieces (8) in order to prevent that slit filling, not shown and made of a synthetic material or another suitable material, from falling out of the transmission slits (7) when the drilling device (1) becomes deformed due to strong torsional forces or during steering movements.
The steering head (9) with a sloping surface is connected to the housing (2) without rotational play in such a way that flat areas (10) are retained by corresponding projections in the housing (2). The steering head (9) is secured against axial displacement by means of a pin gripping through a borehole (11). A lip seal (13) that prevents drilling fluid directed to the steering head (9) via the borehole (5) from passing into the chamber (6) for the transmitter (14) is arranged at a projection (12) of the steering head (9).
The transmitter (14) has a cylindrical housing whose outer diameter is smaller than the inner diameter of the chamber (6) by approximately 5 mm. A buffer (15) is arranged at the end of the transmitter (14) that faces the steering head (9), and an impact-damping buffer (16) is arranged at the end facing the rear end (3) of the housing (2).
The buffers (15, 16) consist preferably of silicone rubber with a Shore A hardness of 15 to 30; however, they may also consist of other impact-damping elastomers. In order to assure the deformability in the axial and radial direction, the buffers (15, 16) are provided with annular grooves (17) and axial boreholes (18). At least the axial borehole (18) in the buffer (15) has an undercut (19) into which a head (20) of a pin (21), connected to the transmitter (14), grips, whereby the buffer (15) is securely held in the axial direction. The axial extent of the undercut (19) is greater than that of the head (20), so that a free space remains into which a pulling hook can be introduced after the steering head (9) has been removed, so that the transmitter (14) can be drawn from the chamber (6) by means of the pulling hook.
At least the buffer (16) is connected to the transmitter (14) without rotational play and has a longitudinal groove (22) into which a projection in the form of a screw (23) grips at the housing (2). In this way, the transmitter (14) assumes with respect to the housing (2) a defined position which does not change during its operation. Nonetheless, this fixation in position is such that neither axial nor radial accelerations are transferred to the transmitter (14).
In order to be able to introduce the transmitter (14) into the chamber (6) in such a way that the screw (23) grips into the longitudinal groove (22), a transverse slit (24) is arranged at the head (20), so that the transmitter (14) can be turned by means of a screwdriver which is introduced into the slit (24), in order to align the longitudinal groove (22) and the screw (23) with each other.
Adjacent to the buffers (15, 16), impact-damping, narrow guide rings (25, 26), whose outer diameter essentially coincides with the inner diameter of the chamber (6) and which serve to guide the transmitter (14) inside the housing (2), are arranged on the housing of the transmitter (14). In case the housing (2) is deformed, the guide rings (25, 26) prevent radial accelerations from being transferred to the transmitter (14).
Two cylindrical batteries (27) are arranged coaxially in a battery compartment (31) of the transmitter (14). It is also possible that only one or more than two batteries may be involved. Between these batteries (27) and on both sides thereof, additional annular buffers (28), also preferably made of silicone rubber with a Shore A hardness of 15 to 30 are arranged which serve to prevent the transfer of particularly high acceleration forces to the batteries (27). In this case, contact springs (30) serve for the contact transfer from the batteries (27) to the electronic components arranged in the housing of the transmitter (14).
In the embodiment according to FIG. 1, the transmitter (14) inside the drilling device is secured against turning by means of a screw (23) that grips into a groove (22). Another embodiment of the very important fixing of the transmitter (14) at the steering head (9) so that it is secured against turning is shown in FIG. 3 and consists of a torsionally elastic guide rod (32) that engages with a buffer (15) that connects the transmitter (14) to the steering head (9).
For this purpose, the buffer (15) has the axial borehole (18).
The connection of the! steering head (9) and! rod (32), may, for example, take place via a tab (33) which grips into a front groove (35) at the steering head (9). By means of its cross section, the tab (33) may be secured against being dislodged. The connection of the! rod (32) and! transmitter (14) may take place via a T-tongue (34) at the rod (32) which grips into a T-groove (36) at the transmitter (14). It is important that the T-groove (36) at the transmitter (14) be laid out in such a way that at the front, the rod (32) has sufficient axial play in this groove (36). The axial play must be greater than the maximally resulting range of elasticity of the buffers (15, 16). Since the rod (32) is attached at the transmitter via the T-tongue (34) and via the tab (33) at the steering head (9), the entire transmitter (14) can be pulled out of the axial borehole by means of the steering head (9). No additional tools, such as a pulling hook or screwdriver, are required for extraction or introduction purposes.
Since the rod (32) is torsionally elastic, no hard blows, as may occur, for example, during the hooking of the steering head (9), will be transferred to the transmitter (14). The rod (32) may preferably be pushed from the side into the T-groove at the transmitter. The buffer (15) sits loosely on the rod (32), so that the transmitter can oscillate freely. The buffers (15, 16) require no longitudinal grooves, since there is no screw (23) gripping therein serving to secure against turning.
The invention is not limited to the example of the drilling device shown, driven in a rotating and impacting manner by means of drill pipes, wherein drilling fluid is directed to the steering head. Rather, the invention may also be used in connection with a pile driver drilling device, operating in a pounding manner, as described, for example, in German Patent No. 2 157 259. In the case of a relatively small axial extent of the transmitter and a corresponding diameter of the drilling device, the transmitter may also be completely embedded in the impact-damping buffer, which may be removed in a problem-free manner for purposes of repair or maintenance. | Arrangement of an impact-sensitive device in a housing, particularly a transmitter for locating a drilling device located in a borehole in the ground, wherein the device is maintained within same by means of at least one impact-damping buffer at least in the main direction of impact and at a distance from the wall of a chamber accommodating the device. | 4 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of application Ser. No. 09/565,862, filed May 5, 2000, pending, which is a continuation of application Ser. No. 08/736,586, filed Oct. 24, 1996, now U.S. Pat. No. 6,133,638, issued Oct. 17, 2000, which is a divisional of application Ser. No. 08/578,493, filed Dec. 22, 1995, now U.S. Pat. No. 5,686,318, issued Nov. 11, 1997.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates generally to die-to-insert interconnections and, more specifically, to a method of forming a permanent die-to-insert electrical connection for a semiconductor die assembly by diffusing gold bumps on the insert into the bond pads of the die using relatively low elevated temperatures and low levels of constant force during the extended time of a burn-in process.
[0004] 2. State of the Art
[0005] Currently, there are three primary chip-level interconnection technologies in practice. They include wirebonding (WB), Tape Automated Bonding (TAB), and Controlled Collapse Chip Connection (C4). The method used to bond the interconnections is dependent upon the number and spacing of input/output (I/O) connections on the chip and the insert (i.e., substrate) as well as permissible cost.
[0006] WB is the most common chip-bonding technology because the required number of chip connections in many products can be accomplished in addition to providing the lowest cost per connection. WB is generally employed to electrically connect chips to the inner ends of the leads of a lead frame, the assembly subsequently being packaged as by transfer molding of a plastic package. For chips requiring more than 257 but less than 600 connections, TAB may be used. TAB employs lead frames of a finer pitch mounted on an insulative carrier tape which is integrated into the chip package. The C4 process, however, is capable of creating up to 16,000 connections per chip (or partial wafer), potentially meeting the demand for any number of connections that the die or partial wafer design dictates.
[0007] When C4 bonding is employed, the entire surface of the chip is normally covered with bond pads for the highest possible I/O count. Solder bumps are deposited on wettable metal terminals (bond pads) on the chip, and a matching footprint of solder-wettable terminals is located on the substrate. Both the bond pads and the terminals must be treated with solder flux. Moreover, the solder bumps must be constrained from completely collapsing (or flowing out onto the substrate bonding site) by using thick-film glass dams, or stops. The tendency for the solder to flow on the chip is contained by a special bonding pad metallurgy that consists of a circular pad of evaporated chromium, copper, and gold. The bond pad metallurgy is then coated by evaporation with, for example, 5Sn-95Pb or 2Sn-98Pb, to a thickness of 100 to 125 μm. Finally, the upside-down chip or die (flip-chip) is aligned to the substrate, and all chip-to-substrate conductive paths are made simultaneously by reflowing the solder.
[0008] The numerous process steps and extensive prebond preparation associated with C4 makes it an expensive bonding method. Moreover, because of the expense added by the C4 process, bumping the chip has been avoided. In the Very Large Scale Integration (VLSI) era, however, the expense has been necessary to obtain the required number of connections.
[0009] As disclosed in U.S. Pat. No. 5,435,734 to Chow, pressure contact interconnect methods are also known in the art. Pressure contacts are not actually bonded but rather form a continuous contact using a material deformation concept such as a metal spring or an elastic retainer. For example, two gold bumps (on chip and substrate) may be joined by a conductive rubber contact embedded in a polyamide carrier. However, this is a mechanically created connection and is, therefore, not as desirable as metallurgical bonding techniques for economic-as well as reliability-associated reasons.
[0010] Furthermore, all of the previously mentioned methods of forming chip-to-substrate interconnections are typically effected after a burn-in operation is performed on the chip to determine if the chip is defective. For burn-in, a chip is typically placed in a multi-chip carrier in resiliently biased or other temporary connection to a burn-in die or substrate (also called an insert) having circuit traces and contacts for electrical testing of the chip. During the burn-in process, the chips are generally subjected to electrical impulses and elevated temperatures (on the order of 125-150° C.) for extended periods of time, usually 24-48 hours, depending upon the chip and the characterization protocol. Low-temperature cycling to as low as −50° C. may also be employed on occasion, particularly for chips being qualified to military specifications. However, this is not common for chips destined for use in commercial applications.
[0011] If not proven defective, the chip is removed from its test fixture after burn-in and is then permanently attached to a substrate by means known in the art, such as those previously mentioned. Alternatively, the chip may be wirebonded to a lead frame or TAB-bonded to a taped lead frame, as known in the art, depending upon the ultimate application for the chip and preferred packaging for that application. In any case, burn-in connections and permanent operational connections are effected in the prior art in two distinct and different operations. While it would be possible to form permanent die-to-insert connections before burn-in, this would increase processing time and cost. It is known to package single die before burn-in, such as with wire- or TAB-bonded lead frame-mounted, plastic-packaged dice (e.g., DIP, ZIP), but such arrangements are not suitable for multi-chip modules (MCM's) such as single in-line memory modules (SIMM's) where failure of a single die will result in scrapping of the module.
[0012] Thus, it would be advantageous to provide an economical method of chip-to-substrate interconnection that is capable of keeping up with the ever-increasing requirements for more I/O connections per chip, does not require all of the preparation and process steps associated with C4 chip interconnections such as application of flux and the use of thick-film glass substrate dams, and removes at least one major step from the manufacturing process through use of a one-step chip-to-substrate electrical connection technique suitable for both burn-in and ultimate first-level packaging of a chip.
[0013] Additional non-C4 ball- or bump-type chip-to-substrate electrical interconnect systems exist in the art, as disclosed in U.S. Pat. Nos. 5,451,274; 5,426,266; 5,369,545; 5,346,857; and 5,341,979. Such systems achieve electrical connections through use of relatively complex and sophisticated apparatus and process methodology, and thus are not suitable for use during chip burn-in in a carrier or other fixture.
[0014] Temporary chip-to-burn-in die or insert connections are also known in the art and exemplified by the disclosures of U.S. Pat. Nos. 5,440,241; 5,397,997; and 5,249,450. None of the foregoing patents, however, discloses a methodology for forming suitably permanent die-to-substrate electrical connections during burn-in.
[0015] It is known in the electronics art to employ diffusion bonding to effect electrical connections between two or more substrates or circuit boards; U.S. Pat. No. 5,276,955 discloses such a process. However, diffusion bonding as known in the art is generally effected at relatively high temperatures just below the eutectic or peritectic temperatures of the bonding alloy, and for relatively short periods of time, such as one or two hours. Thus, state-of-the-art diffusion bonding as known to the inventors has no legitimate application to making chip-to-insert connections.
BRIEF SUMMARY OF THE INVENTION
[0016] According to the invention, a method for forming a permanent chip-to-insert interconnection is herein disclosed. Gold bumps are attached to ends of conductive circuit traces on one side or the other of a nonelectrically conductive substrate, or even the exposed ends of internal conductors, by which electrical testing of a chip during burn-in is effected. As used herein, it should be understood that the term “gold” includes not only elemental gold, but gold with other trace metals and in various alloyed combinations with other metals as known in the semiconductor art. Typically, the die has bond pads on one surface (commonly termed the “front” or “active” surface) formed of aluminum or an aluminum alloy. The bond pads are arranged as a mirror image of the gold bumps located on the surface of the substrate. Thus, when the bond pads are placed on top of the gold bumps, they are in substantial alignment with each other.
[0017] The substrate material is selected such that the coefficient of thermal expansion (CTE) is similar to that of the die or semiconductor chip. This assures that both the substrate and the die expand and contract in a similar manner when subjected to elevated temperatures during a burn-in process so that the bond pads on the die will stay in relatively precise alignment with the gold bumps on the substrate, producing little or no shear force between any bond pad and its corresponding bump. By way of example only, the substrate may be comprised of Mullite, a ceramic material such as 203 aluminum oxide, or any other material known in the art that has a CTE similar to that of the die.
[0018] By applying a force to the die as it is located above and parallel to the plane of the substrate, the bond pads and gold bumps are pressed together. The die/substrate assembly is then heated to effect a bond between the conductive paths of the two components of the assembly. The heat applied, however, is not sufficient to melt the gold bumps or even to approach the eutectic or peritectic threshold of the gold, but only to the extent necessary to diffuse the gold to form a permanent aluminum/gold bond between the gold bump and the aluminum bond pad. Thus, the gold from the gold bump diffuses into the aluminum bond pads of the die.
[0019] The method herein disclosed is preferably performed during the burn-in process. During the heating cycle, the temperature can be set or cycled to provide the necessary diffusion energy to form the aluminum/gold bond. Moreover, the chips may be placed in chip carriers which utilize a spring or other biasing member to press the bond pads of the semiconductor die and the gold bumps of the substrate (burn-in die, insert) together. The assemblies are then subjected to selected temperatures for a selected period of time, the combination of temperature and time promoting diffusion of the gold into the aluminum bond pads of the die. Contrary to prior art diffusion bonding methods, the diffusion temperature of the present invention is markedly lower, and the diffusion time markedly longer. Of course, were this not the case, the semiconductor die circuitry, if not the die itself, would be damaged and its performance characteristics altered.
[0020] Since there is an initial biased electrical contact as soon as the die under test (DUT) is secured against the gold bumps of the substrate in the carrier, electrical testing with elevated potentials as well as thermal testing of the die may commence immediately and continue while the permanent, bump-to-pad diffusion bond is created. Each die that fails during the burn-in process may then simply be discarded at the termination of burn-in along with its attached substrate for recovery of the precious metals. Alternatively, the die may be mechanically removed and a new die attached to the die location on the substrate. It has been found to be, in terms of processing time versus ultimate yield, less expensive to form a permanent chip-to-substrate attachment during burn-in than to perform burn-in followed by a permanent chip attachment to a second substrate, even if some dice have to be pulled as defective or substandard and replaced.
[0021] An added advantage of the method of chip-to-substrate interconnection of the present invention is its capability of keeping up with the requirements for ever-increasing numbers of I/O connections, the reduction of process and preparation steps in comparison to C4 bonding and other flip-chip bonding systems known in the art, and the deletion of at least one major step from the fabrication, testing and packaging sequence.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0022] The present invention will be more fully understood and appreciated by those of ordinary skill of the art by a review of this specification, taken in conjunction with the appended drawings, wherein:
[0023] [0023]FIG. 1 is a side view of a semiconductor die contained against a gold-bumped substrate in a burn-in fixture in accordance with the method of the present invention;
[0024] [0024]FIG. 2 is a partial top perspective view of a gold-bumped substrate showing circuit traces thereon;
[0025] [0025]FIG. 3 is a schematic view of the active surface of a high bond pad density semiconductor die suitable for use in accordance with the present invention;
[0026] [0026]FIG. 4 is a schematic top view of a gold-bumped burn-in substrate suitable for use in accordance with the present invention;
[0027] [0027]FIG. 5 is an exploded side view of the semiconductor die, burn-in substrate and burn-in fixture of the embodiment shown in FIG. 1; and
[0028] [0028]FIG. 6 is an end view of the semiconductor device and burn-in fixture shown in FIG. 1.
DETAILED DESCRIPTION OF THE INVENTION
[0029] Referring to FIG. 1, a side view of a semiconductor die assembly 10 positioned in a burn-in fixture 12 is shown. The term “die” as used herein may denote a single die (chip) from a wafer or a plurality of dies, up to an entire wafer if wafer-scale integration is employed for the unit under test.
[0030] The semiconductor die assembly is comprised of a nonelectrically conductive substrate 14 (also commonly termed an insert or burn-in die in the prior art) on which a plurality of gold bumps 16 is formed by means known in the art. The bumps 16 are located at the ends of circuit traces 17 extending to the periphery of the substrate 14 for electrical testing during burn-in (see FIG. 2). One suitable means of forming gold bumps on substrate 14 is through use of a thermosonic gold wire bonding apparatus as known in the art and commercially available from Kulicke and Soffa Industries of Willow Grove, Pa. The bumps may be coined to a desired configuration after deposition, as known in the art. (See U.S. Pat. Nos. 5,397,997 and 5,249,450 for a discussion of various bump-forming techniques.) The preferred compositions of the gold bumps employed in the present invention may comprise 99.99% pure gold (Au) bond wire, as well as Be- or Cu-doped Au, or other Au-based alloys as known in the art. Aluminum (Al) wire may also be used to form the bumps, using ultrasonic apparatus as known in the art.
[0031] A semiconductor die 18 with active and optionally passive components, as well as circuit traces, vias and other conductive paths as known in the art, is positioned on top of the gold bumps 16 . The substrate 14 is placed in the base 20 of the burn-in fixture 12 with the gold bumps 16 facing upwardly, away from the base 20 . The die 18 is aligned with the substrate 14 (the die and substrate planes being mutually parallel and die and substrate electrical contacts being coincident) and a lid or cover 22 is placed on top of the die 18 .
[0032] As better seen in FIGS. 3 and 4, the die 18 has a plurality of bond pads 13 in the same configuration as the gold bumps 16 on the substrate 14 . Thus, when the die 18 is placed on the substrate 14 , the bond pads 13 and the gold bumps 16 match. Moreover, for alignment purposes, one gold bump 15 may be offset from the rest, leaving a space 19 on the substrate surface, and one bond pad 13 ′ offset from the rest of the bond pads 13 , leaving a space 21 corresponding to the space 19 . Thus, correct rotational orientation of the die 18 relative to the substrate 14 can be easily ascertained. Spaces 19 and 21 may, of course, be eliminated and a bump 16 and bond pad 13 merely offset in alignment. Of course, other alignment methods known in the art, such as marking the components for alignment or creating a die/substrate interconnect pattern which can only be mated in one orientation, may also be employed.
[0033] The bridge clamp 24 of the burn-in fixture 12 comprises an upper plate 26 having a first end 28 and a second end 30 to which perpendicularly extending legs 32 and 34 are attached about their proximal ends 36 and 38 , respectively. The legs 32 and 34 have anchors 40 and 42 resiliently disposed at the distal ends 44 and 46 of the legs 32 and 34 , respectively. Spaced upwardly from the anchors 40 and 42 are stop members 48 and 50 extending outwardly from legs 32 and 34 .
[0034] Attached to the underside 52 of the bridge clamp 24 is a biasing member 54 . The biasing member 54 may be comprised of spring steel and configured as a leaf spring, coil spring or belleville spring, or be formed of some other resilient material known in the art and capable of withstanding the elevated burn-in temperatures, such as a silicone-based elastomers. The biasing member 54 should also be designed to apply a selected amount of force to the back side of die 18 when the burn-in fixture 12 is closed, within a broad range capable of providing sufficient force for bonding contact but not excessive, damaging force to the die 18 , the bumps 16 , or the substrate 14 . The biasing member 54 as shown is held in position by projections 51 and 53 extending from the underside 52 of the bridge clamp 24 . The projections 51 and 53 are angled inwardly toward one another and provide for an abutment of the biasing member 54 . Other connection means are possible and contemplated, including a tab or extension of biasing member 54 sliding into slots in bridge clamp 24 .
[0035] The burn-in fixture 12 is designed to apply pressure to the interfaces 56 between the gold bumps 16 and the die 18 transversely to the planes of the die 18 and substrate 14 . As shown in FIG. 5, the anchors 40 and 42 are deflected and inserted through slots 58 and 60 . The stop members 48 and 50 prevent the legs 32 and 34 from being inserted too far into the slots 58 and 60 and thus prevent excessive force from being applied by the biasing member 54 on the lid or cover 22 .
[0036] When the anchors 40 and 42 are properly secured to the bottom 62 of the base 20 , a predetermined amount of force is applied by the biasing member 54 to the surface of the lid or cover 22 . Because the lid or cover 22 substantially covers the die 18 and is of sufficient strength to resist bending or other deflection (FIGS. 1 and 6), the lid or cover 22 provides uniform pressure across the surface 64 of the die 18 . Moreover, the pressure may be sufficient to ensure that all of the gold bumps 16 are held in contact with the bond pads 13 on the surface 64 of the die 18 .
[0037] [0037]FIG. 6 shows the right side end view of the embodiment of FIG. 5. As shown, the biasing member 54 extends over a substantial portion of the lid or cover 22 so that pressure is evenly applied to the top 57 of the lid or cover 22 . Because of the even pressure applied to the lid or cover 22 and subsequently between the gold bumps 16 and the bond pads 13 , diffusion between all gold bumps 16 and all bond pads 13 under burn-in temperatures can occur substantially simultaneously.
[0038] Because of the potential for inherent variation in the height of each gold bump 16 , some gold bumps 16 may not initially be in contact with the bond pads 13 of the substrate 14 . While solvable through a coining operation as previous mentioned, such an additional process step (if not performed during bump application) may desirably be omitted. Dimensional variation of the substrate-to-die electrical contacts presented substantial problems with the use of prior art burn-in substrates or inserts employing hard, electroplated contact bumps of nonporous nickel. However, as the gold bumps 16 that are in initial contact with the bond pads 13 relax in height slightly as they are compressed during assembly, the distance between the die 18 and the substrate 14 will decrease under the force applied by biasing member 54 until those gold bumps 16 not initially in contact with the bond pads 13 do, in fact, contact and diffuse into the bond pads 13 .
[0039] The semiconductor die assembly 10 that is contained in the burn-in fixture 12 is subjected to heat during a burn-in process to elevate the assembly 10 to a predetermined temperature above ambient, typically 125-150° C. as previously noted. The burn-in temperature, in combination with the relatively slight temperature elevation of the die due to electrical testing during burn-in, is sufficient to cause the gold of the gold bumps 16 to diffuse into the bond pads 13 of the die 18 , but is not high enough to cause the gold in the gold bumps 16 to liquify or to cause damage (beyond the normal purpose of a burn-in to identify defective DUT's) to the DUT. The elevated temperature is maintained for a selected period of time, until burn-in is completed and diffusion of the gold into the bond pads 13 has formed a permanent bond. It should be noted that certain semiconductor devices have recently been developed for operation at elevated temperatures, such as 180° C. or slightly higher in applications such as aerospace or oil and gas exploration. Burn-in for such chips would naturally be conducted at temperatures higher than 150° C., but still far short of the melting point of gold or most gold alloys. Thus, diffusion bonding according to the present invention would have equal utility for such chips.
[0040] The time required for sufficient diffusion bonding of the gold bumps of elemental gold or a given alloy to the bond pads can readily be determined, both mathematically and empirically, based on the bump metal or alloy employed and the temperature selected during which the die is biased against the adjacent, parallel substrate. The higher the temperature, the faster the diffusion rate. Thus, for a higher temperature, less time is required for the desired diffusion to occur for any given bump metal.
[0041] While the present invention has been described in terms of certain preferred embodiments, it is not so limited, and those of ordinary skill in the art will readily recognize and appreciate that many additions, deletions and modifications to the embodiments described herein may be made without departing from the scope of the invention as hereinafter claimed. For example, a plurality of dice may be simultaneously bonded to a like plurality of substrates in a carrier during burn-in; while the term gold “bumps” has been employed, that term may encompass gold balls, cylinders, cuboids, pyramids or cones (including truncated such structures); the term “bond pad” is intended to include and encompass all suitable terminal structures to which a diffusion bond may be made, including both elevated and recessed bond pads as well as flat, concave or convex bond pads and other terminal structures; and bond pads may be formed of gold-compatible materials other than aluminum. | The invention disclosed herein is a semiconductor die assembly and method of making the same having a die and insert substrate that are electrically interconnected by diffusing gold bumps attached to the connecting surface of the substrate to aluminum-based bond pads on the die to form a permanent die-to-insert connection. The process for diffusing the gold bumps into the bond pads preferably occurs during a burn-in process wherein pressure and heat are applied to the die/substrate assembly without melting the gold bumps until a permanent die-to-insert substrate connection is properly made. | 7 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of application Ser. No. 10/152,535 filed on May 20, 2002 and claims priority under 35 U.S.C. 119 of Danish application no. 0317/97 filed on Mar. 20, 1997, of U.S. provisional application No. 60/041,390 filed on Mar. 27, 1997 and the benefit of application Ser. Nos. 09/045,038, 09/836,496 and 10/152,535 filed on Mar. 20, 1998, Apr. 17, 2001 and May 20, 2002 respectively, in the U.S. is claimed under 35 U.S.C. 120, the contents of all of which are fully incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The present invention relates to zinc free insulin crystals having a diameter below 10 μm and to therapeutic powder formulations suitable for pulmonary administration comprising such insulin crystals.
BACKGROUND OF THE INVENTION
[0003] Diabetes is a general term for disorders in man having excessive urine excretion as in diabetes mellitus and diabetes insipidus. Diabetes mellitus is a metabolic disorder in which the ability to utilize glucose is more or less completely lost. About 2% of all people suffer from diabetes.
[0004] Since the introduction of insulin in the 1920's, continuous strides have been made to improve the treatment of diabetes mellitus. To help avoid extreme glycaemia levels, diabetic patients often practice multiple injection therapy, whereby insulin is administered with each meal.
[0005] Insulin is usually administrated by s.c. or i.m. injections. However, due to the adherent discomfort of injections alternative ways of administration such as nasal and pulmonary has been extensively investigated. For a review on alternative routes of administration of insulin, see Danielsen et al. New routes and means of insulin delivery, in: Childhood and Adolescent Diabetes (Ed. Kelnar), Chapman & Hall Medical, London 1994, pp. 571-584.
[0006] In order to circumvent injections, administration of insulin via the pulmonary route could be an alternative way to provide absorption profiles which mimic the endogenous insulin without the need to inject the insulin.
DESCRIPTION OF THE BACKGROUND ART
[0007] Administration of insulin via the pulmonary route can be accomplished by either an aqueous solution or a powder preparation. A description of the details can be found in several references, one of the latest being by Niven, Crit. Rev. Ther. Drug Carrier Sys, 12(2&3): 151-231 (1995). One aspect covered in said review is the stability issue of protein formulations, aqueous solutions being less stable than powder formulation. So far, all powder formulations have been described as mainly amorphous.
[0008] A review of the permeation enhancers useful for the promotion of trans-mucosal absorption is found in Sayani et al., Crit. Rev. Ther. Drug Carrier Sys, 13(1&2): 85-184 (1996).
[0009] Patton et al., Inhale Therapeutic Systems, PCT WO 95/24183, claim a method for aerosolising a dose of insulin comprising providing the insulin as a dry powder dispersing an amount of the dry powder in a gas stream to form an aerosol capturing the aerosol in a chamber for subsequent inhalation.
[0010] It has been found that when insulin is combined with an appropriate absorption enhancer and is introduced into the lower respiratory tract in the form of a powder of appropriate particle size, it readily enters the systemic circulation by absorption through the layer of epithelial cells in the lower respiratory tract as described in U.S. Pat. No. 5,506,203. The manufacturing process described in said patent, comprising dissolution of insulin at acid pH followed by a pH adjustment to pH 7.4 and addition of sodium taurocholate before drying the solution by vacuum concentration, open drying, spray drying, or freeze drying, results in a powder composed of human insulin and absorption enhancer. The powder is characterized as mainly amorphous determined under a polarized light microscope. The desired particle size distribution is achieved by micronizing in a suitable mill, such as a jet mill, and the components may be mixed before or after micronizing. The biological effect of the powder obtained according to the methods described in this patent is only seen in the presence of a substantial amount of enhancer.
[0011] Platz et al., Inhale Therapeutic Systems, PCT WO 96/32149, describes spray drying of zinc insulin from a solution containing mannitol and a citrate buffer, pH 6.7. The inlet temperature is 120 to 122□C, the outlet temperature 80-81□C. The mass median aerodynamic diameter, MMAd, of the obtained insulin particles was determined to 1.3 to 1.5 μm.
[0012] In his thesis, “Insulin Crystals”, Munksgaard Publisher 1958, p. 54-55, Schlichtkrull describes crystallisation of zinc free, recrystallised porcine insulin from a solution comprising 0.01 M sodium acetate and 0.7% ˜0.12 M sodium chloride and 0.1% methyl-parahydroxybenzoate and using a pH of 7.0. The crystals obtained were 10-50 μm rhombic dodecahedral crystals showing no birefringence.
[0013] Jackson, U.S. Pat. No. 3,719,655 describes a method of purification of crude porcine and bovine insulin by crystallisation. Zinc free crystals of insulin are obtained by crystallisation at pH 8.2 (range 7.2-10) in the presence of 0.5 M (range 0.2 M-1 M) of a sodium, potassium, lithium or ammonium salt. Crystallisation is achieved by addition of 1 N alkali metal hydroxide or 1 N ammonia to a solution of crude insulin in 0.5 N acetic acid to a pH of 8.2 is obtained. Alternatively, crystallisation is achieved in an aqueous solution of impure insulin at pH 8.2 by addition of solid sodium chloride to a concentration of sodium ions of 0.45 M. The crystals appear in the octadecahedral or dodecahedral forms, i.e. crystals belonging to the cubic crystal system.
[0014] Baker et al., Lilly, EP 0 709 395 A2 (filed Oct. 31, 1994) describe a zinc free crystallisation process for Lys B28 -Pro B29 human insulin characterised by adjustment of the pH of a strongly buffered acid solution containing metal cations or ammonium ions and a preservative with metal hydroxide or ammonia to a value between 8.5 and 9.5.
[0015] The known methods for the manufacture of insulin particles of the desired size for pulmonary administration are cumbersome, generates problems with insulin dust and the investments in equipment are large. Furthermore, insulin is exposed to conditions where some denaturation is likely to take place. Thus WO 96/32149 disclose spray drying in a temperature range of 50□C to 100□C, followed by milling of the particles to achieve to desired particle size.
[0016] Furthermore, the known powder formulations for pulmonary administration which have been described as mainly amorphous have a tendency to associate into aggregates in the dry powder.
DESCRIPTION OF THE INVENTION
[0000] Definitions
[0017] The expression “enhancer” as used herein refers to a substance enhancing the absorption of insulin, insulin analogue or insulin derivative through the layer of epithelial cells lining the alveoli of the lung into the adjacent pulmonary vasculature, i.e. the amount of insulin absorbed into the systemic system is higher than the amount absorbed in the absence of enhancer.
[0018] In the present context the expression “powder” refers to a collection of essentially dry particles, i.e. the moisture content being below about 10% by weight, preferably below 6% by weight, and most preferably below 4% by weight.
[0019] The diameter of the crystals is defined as the Martin's diameter. It is measured as the length of the line, parallel to the ocular scale, that divides the randomly oriented crystals into two equal projected areas
BRIEF DESCRIPTIONS OF THE INVENTION
[0020] It is an object of the present invention to provide an insulin powder suitable for pulmonary delivery which has a reduced tendency to associate into aggregates in the dry powder compared to the pulmonary insulin particles described in the prior art.
[0021] According to the present invention this object has been accomplished by providing zinc free insulin crystals having a diameter below 10 μm.
[0022] The crystals of the present invention furthermore exhibit a better stability profile than powders of essentially the same composition prepared by spray drying, freeze-drying, vacuum drying and open drying. This is probably due to the amorphous state of powders prepared by the other methods described. By this means it is possible to store the powder formulations based on the crystals of the present invention at room temperature in contrary to human insulin preparations for injections and some amorphous insulin powders without stabilizing agent which have to be stored between 2□C to 8□C.
[0023] Furthermore, therapeutical powder formulations comprising the insulin crystals of the invention elucidates better flowing properties than corresponding amorphous powder formulations.
Preferred Embodiments
[0024] The zinc free insulin crystals of the invention are advantageously provided in a crystal structure belonging to the cubic crystal system, preferably in the octadecahedral or dodecahedral crystal forms, since these crystal forms result in readily soluble product having excellent flowing properties.
[0025] The diameter of the insulin crystals is advantageously kept in the range of 0.2 to 5 μm, preferably in the range of 0.2 to 2 μm, more preferably in the range of 0.5 and 1 μm, to ensure high bioavailability and suitable profile of action, see PCT application No. WO 95/24183 and PCT application No. WO 96/32149.
[0026] In a preferred embodiment the insulin used is selected from the group consisting of human insulin, bovine insulin or porcine insulin, preferably human insulin.
[0027] In another preferred embodiment the insulin used is selected from the group consisting of rapid-acting insulins, preferably des(B30) human insulin, Asp B28 human insulin or Lys B28 Pro B29 human insulin.
[0028] In another preferred embodiment the insulin used is an insulin derivative, preferably selected from the group consisting of B29-N ε -myristoyl-des(B30) human insulin, B29-N ε -palmitoyl-des(B30) human insulin, B29-N ε -myristoyl human insulin, B29-N ε -palmitoyl human insulin, B28-N ε -myristoyl Lys B28 Pro B29 human insulin, B28-N ε -palmitoyl Lys B28 Pro B29 human insulin, B30-N ε -myristoyl-Thr B29 Lys B30 human insulin, B30-N ε -palmitoyl-Thr B29 Lys B30 human insulin, B29-N ε -(N-palmitoyl-γ-glutamyl)-des(B30) human insulin, B29-N ε -(N-lithocholyl-γ-glutamyl)-des(B30) human insulin, B29-N ε -(ω-carboxyheptadecanoyl)-des(B30) human insulin and B29-N ε -(ω-carboxyheptadecanoyl) human insulin, more preferably Lys B29 (N-ε acylated) des(B30) human insulin.
[0029] The insulin derivatives has a protracted onset of action and may thus compensate the very rapid increase in plasma insulin normally associated with pulmonary delivery. By carefully selecting the type of insulin, the present invention enables adjustment of the timing and to obtain the desired biological response within a defined time span.
[0030] In order to avoid irritation of the lungs and to eliminate immunological reactions, the employed insulin is preferably insulin which has been purified by chromatography, such as MC insulin (Novo), Single Peak insulin (E. Lilly) and RI insulin (Nordisk).
[0031] In a preferred embodiment the zinc free insulin crystals according to the invention further comprise a stabilizing amount of a phenolic compound, preferably m-cresol or phenol, or a mixture of these compounds.
[0032] The present invention is furthermore concerned with a therapeutic powder formulation suitable for pulmonary administration comprising the zinc free crystals described above.
[0033] In a preferred embodiment this therapeutic powder formulation further comprises an enhancer which enhances the absorption of insulin in the lower respiratory tract.
[0034] The enhancer is advantageously a surfactant, preferably selected from the group consisting of salts of fatty acids, bile salts or phospholipids, more preferably a bile salt.
[0035] Preferred fatty acids salts are salts of C 10-14 fatty acids, such as sodium caprate, sodium laurate and sodium myristate.
[0036] Lysophosphatidylcholine is a preferred phospholipid.
[0037] Preferred bile salts are salts of ursodeoxycholate, taurocholate, glycocholate and taurodihydrofusidate. Still more preferred are powder formulations according to the invention wherein the enhancer is a salt of taurocholate, preferably sodium taurocholate.
[0038] The molar ratio of insulin to enhancer in the powder formulation of the present invention is preferably 9:1 to 1:9, more preferably between 5:1 to 1:5, and still more preferably between 3:1 to 1:3.
[0039] The powder formulations of the present invention may optionally be combined with a carrier or excipient generally accepted as suitable for pulmonary administration. The purpose of adding a carrier or excipient may be as a bulking agent, stabilizing agent or an agent improving the flowing properties.
[0040] Suitable carrier agents include 1) carbohydrates, e.g. monosaccharides such as fructose, galactose, glucose, sorbose, and the like; 2) disaccharides, such as lactose, trehalose and the like; 3) polysaccharides, such as raffinose, maltodextrins, dextrans, and the like; 4) alditols, such as mannitol, xylitol, and the like; 5) inorganic salts, such as sodium chloride, and the like; 6) organic salts, such as sodium citrate, sodium ascorbate, and the like. A preferred group of carriers includes trehalose, raffinose, mannitol, sorbitol, xylitol, inositol, sucrose, sodium chloride and sodium citrate.
[0041] The crystals of the present invention are advantageously produced according to the following procedure:
providing a solution of insulin having a pH between 7.0 and 9.5; mixing said solution with a solution of a salt of an alkali metal or an ammonium salt; and recovering the formed crystals.
[0045] The salt of an alkali metal or ammonium is preferably selected from the group consisting of the hydrochloride or acetate of sodium, potassium, lithium or ammonia, or mixtures thereof, more preferably sodium acetate.
[0046] In order to suppress the solubility of the crystals formed, the solution of insulin and/or the solution of a salt of an alkali metal or an ammonium salt preferably comprises a water miscible organic solvent in an amount which corresponds to 5 to 25% (v/v) in the solution obtained after mixing.
[0047] The water miscible organic solvent is preferably selected from the group consisting of ethanol, methanol, acetone and 2-propanol, more preferably ethanol.
[0048] A very uniform distribution of crystal sizes and crystals of the same crystallographic form are obtained when the two solutions are mixed within a period of less than 2 hours, preferably less than 1 hour, more preferably less than 15 minutes, still more preferably less than 5 minutes.
[0049] The crystallisation process by which uniformly sized, small, zinc free crystals is obtained directly, without the use of milling, micronizing, sieving and other dust generating steps, is much to be preferred from the present state of the art in the manufacture of insulin powders for inhalation.
[0050] The concentration of insulin after mixing is preferably between 0.5% and 10%, more preferably between 0.5% and 5%, still more preferably between 0.5% and 2%.
[0051] The concentration of salt after mixing is preferably between 0.2 M and 2 M, more preferably about 1 M.
[0052] The method according to the present invention may further comprise a washing step, in which the crystals obtained are washed with a solution comprising auxiliary substances to be included in the final dry powder, preferably an enhancer and/or a carbohydrate, and optionally comprising 5-25% of an alcohol, preferably ethanol, 5-50 mM of a preservative preferably phenol, and 0.1-2 M of a salt such as sodium acetate.
[0053] This invention is further illustrated by the following examples which, however, are not to be construed as limiting.
EXAMPLE 1
[0000] Crystallisation in 1 M Sodium Acetate.
[0054] 2 g of highly purified human insulin is dissolved in 100 ml 10 mM tris buffer, pH 8.0 in 20% (v/v) of ethanol in water. To this solution is added 100 ml 2 M sodium acetate under stirring. A precipitate forms immediately. After 2 days at room temperature microscopy shows small crystals having a diameter between 0.5 and 1 μm. The crystals are collected by centrifugation at −10□C, washed once with 20 ml ice cold 10% ethanol (v/v) in water, isolated by centrifugation and dried by lyophilization. The obtained crystals are shown in FIG. 1 .
EXAMPLE 2
[0000] Crystallisation in the Presence of Taurocholic Acid Sodium Salt.
[0055] 10 mg of human insulin and 5 mg of taurocholic acid sodium salt are dissolved in 500 μl 10 mM tris buffer, pH 8.0 in 20% (v/v) of ethanol in water. To this solution is added 500 μl 2 M sodium acetate. Microscopy after 1 hour and after 24 hours shows identically appearance of the crystals, i.e. uniformly sized crystals having diameters between 0.5 and 1 μm. The crystals were washed three times with 100 μl 10% (v/v) ethanol in water at −10□C and dried in vacuo. HPLC of the crystals showed that the washings had removed the taurocholic acid sodium salt from the insulin crystals.
EXAMPLE 3
[0000] Crystallisation in the Presence of Tween 80, bis(2-ethylhexyl) Sulfosuccinate Sodium Salt, Chitosan, L-α-lysophosphatidylcholine Myristoyl and Polyoxyethylene Sorbitan Monolaurate.
[0056] Crystallisation was performed as described in Example 2 except that taurocholic acid sodium salt was replaced by 0.6% (w/v) Tween 80, 0.56% (w/v) bis(2-ethylhexyl) sulfosuccinate sodium salt, 0.32% (w/v) chitosan, 0.52% (w/v) L-αlysophosphtidylcholine myristoyl, and 1% (w/v) polyoxyethylene sorbitan monolaurate, respectively. All five examples resulted in uniformly sized crystals having diameters between 0.5 and 1 μm.
EXAMPLE 4
[0057] Crystallisation in 10% (v/v) Ethanol.
[0058] Crystallisation was performed in 10% (v/v) ethanol as described in Example 1, using 4 combinations of pH and concentration of sodium acetate:
4.1: pH 7.5 and 1 M sodium acetate 4.2: pH 7.5 and 1.5 M sodium acetate 4.3: pH 9.0 and 1 M sodium acetate 4.4: pH 9.0 and 1.5 M sodium acetate
[0063] All 4 combinations yielded uniformly sized crystals having diameters between 0.5 and 1 μm.
EXAMPLE 5
[0000] Crystallisation in 15% (v/v) Ethanol.
[0064] Crystallisation was performed in 15% (v/v) ethanol, using 6 combinations of pH and concentration of sodium acetate:
5.1: pH 7.5 and 1 M sodium acetate 5.2: pH 7.5 and 1.5 M sodium acetate 5.3: pH 7.5 and 2 M sodium acetate 5.4: pH 9.0 and 1 M sodium acetate 5.5: pH 9.0 and 1.5 M sodium acetate 5.6: pH 9.0 and 2 M sodium acetate
[0071] All 6 combinations yielded uniformly sized crystals having diameters between 0.5 and 1 μm.
EXAMPLE 6
[0000] Crystallisation in 20% (v/v) Ethanol.
[0072] Crystallisation was performed in 20% (v/v) ethanol using 4 combinations of pH and concentration of sodium acetate:
6.1: pH 7.5 and 1 M sodium acetate 6.2: pH 7.5 and 1.5 M sodium acetate 6.3: pH 7.5 and 2 M sodium acetate 6.4: pH 9.0 and 1 M sodium acetate
[0077] All 4 combinations yielded uniformly sized crystals having diameters between 0.5 and 1 μm.
EXAMPLE 7
[0000] Crystallisation at pH 7.5, 8.0, 8.5 and 9.0 in 20% Ethanol (v/v) Using Slow Addition of Sodium Acetate.
[0078] Crystallisation was performed using solutions as described in Example 1, except that the 2 M sodium acetate was dissolved in 20% (v/v) ethanol in water. The pH of the insulin solutions were adjusted to 7.5, 8.0, 8.5 and 9.0, respectively. The sodium acetate solution was added in aliquots over a period of 2 hours, using 10 min between additions. At all 4 pH values uniformly sized crystals having diameters between 0.5 and 1 μm were obtained.
EXAMPLE 8
[0000] Crystallisation of Lys B29 (ε-myristoyl) des(B30) Human Insulin in the Presence of Taurocholic Acid Sodium Salt.
[0079] 10 mg of Lys B29 (ε-myristoyl) des(B30) human insulin and 5 mg of taurocholic acid sodium salt are dissolved in 500 μl 10 mM tris buffer, pH 8.0 in 20% (v/v) of ethanol in water. To this solution is added 500 μl 2 M sodium acetate. Microscopy after 1 hour and after 24 hours shows identically appearance of the crystals, i.e. uniformly sized crystals having diameters between 0.5 and 1 μm. The crystals were washed once with 300 μl 10% (v/v) ethanol in water at −10□C and dried in vacuo. HPLC of the crystals showed that the washings had removed the palmitoyl-Thr B29 Lys B30 human insulin, B29-N ε -(N-palmitoyl-γ-glutamyl)-des(B30) human insulin, B29-N ε -(N-lithocholyl-γ-glutamyl)-des(B30) human insulin, B29-N ε -(ω-carboxyheptadecanoyl)-des(B30) human insulin and B29-N ε -(ω-carboxyheptadecanoyl) human insulin. | The present invention provides methods and compositions for treating diabetes by administering acylated insulin or an acylated insulin analog via a pulmonary route. The insulin or insulin analog may be in the form of a dry powder or a solution. | 0 |
FIELD OF THE INVENTION
The present invention relates to knitting machines, and in particular to selectors which select which latch needles of a knitting machine are activated in the process of knitting a fabric.
BACKGROUND OF THE INVENTION
Automatic knitting machines use banks of large numbers of closely spaced latch needles to interlock threads in a series of connected loops to produce a knitted fabric. The latch needle is a flat needle generally with a long shaft having, at one end, a small hook with a latch, which latch swivels to open and close the hook.
Generally, in a modem knitting machine, many thousands of latch needles are accurately positioned and maintained in a closely packed parallel array. In the process of knitting a fabric, an activation station activates latch needles by moving them forwards and backwards, parallel to their lengths, so that the hook ends of the activated latch needles move towards and away from threads being woven into the fabric. As a latch needle is moved forwards and backwards, its latch swivels back and forth to alternately open and close the latch needle hook so that the latch needle can catch and hold one of the threads being woven into the fabric, pull it to create a loop of fabric, and then release the thread to repeat the cycle.
In rotary knitting machines the needles in an array are held in a cylindrical geometry and rapidly moved, in a rotary motion, into and out of the activation station. Depending upon the fabric being knitted, different ones of the needles moving through the activation station are activated. In linear knitting machines, latch needles are held in parallel slots in large flat needle beds. The activation station is a type of shuttle that moves rapidly back and forth over the needle bed, activating needles appropriate to the weave of the fabric being knitted.
In both rotary and linear knitting machines, a device called a “selector” determines (hereafter referred to as “selects”) whether a needle in the activation station of the knitting machine is to be activated or not. To prevent a needle from being activated, the selector presses on a small protuberance (hereafter referred to as an “activation fin” or “fin”) on the shaft of the needle. When pressure is applied to the activation fin by the selector, the needle moves away from an activating mechanism of the activator station and is “deactivated”. If the selector does not press on the activation fin, the needle is activated.
The selector presses on the fin of a needle, to deactivate the needle, with a “selector foot”. The selector foot has two operational selection positions. In a deactivate selection position, the selector foot presses on the fin of the needle thereby preventing the needle from being activated when the needle passes through the activation station. In an activate selection position, the selector foot does not press on the fin of the needle, thereby allowing the needle to be activated when the needle passes through the activation station. The selector foot is generally switched between the selection positions by displacing the selector foot by a small linear translation or by rotating the selector foot through a small angle.
When a knitting machine is operating, the selector of the knitting machine is set to an appropriate selection position for each latch needle that passes through the activation station of the knitting machine. If the selection positions for two needles that pass consecutively through the activation station are not the same the selector has to be switched from one selection position to the other. Prior art selectors generally use solenoids or piezoelectric bimorph actuators to effect the displacements necessary to switch a selector foot between selection positions. However, using these types of actuators, the time it takes to switch a selector foot between selection positions is too long to match the rate at which modern knitting machines move needles through activation stations.
In order to improve the speed with which prior art selectors operate, prior art selectors generally comprise a multiplicity of selector feet which are operated in parallel. In a selector operating with one selector foot, a decision to switch or not switch the selection position of the selector foot, hereafter referred to as “setting” the selector foot, has to be made and executed for every needle that moves through an activation station. In a selector with N activation feet on the other hand, each foot has to be set once for every N needles that move through the activation station. If the switching time needed to switch a selector foot between selection positions is τ secs, a selector with one foot can select 1/τ needles/sec, or equivalently, operate at a “decision” frequency of 1/τ Hz. A selector with N selector feet in parallel on the other hand, can select N/τ needles/sec, i.e. operate at a decision frequency of N/τ Hz. Switching times for prior art activation feet are on the order of 10 msecs. By operating approximately 10 activation feet in parallel, prior art selectors are able to operate at decision frequencies of up to about 1000 Hz.
The decision frequencies at which prior art selectors operate limit the rate at which needles can be moved through a knitting machine activation station and therefore limit the rate at which fabric can be produced. In order to increase the rate at which knitting machines produce fabric, it is desirable to have selectors that can operate at frequencies higher than 1000 Hz.
SUMMARY OF THE INVENTION
It is an object of some aspects of the present invention to provide a selector for knitting machines that can operate at decision frequencies substantially higher than 1000 Hz.
A selector, in accordance with a preferred embodiment of the present invention, achieves decision frequencies higher than those of conventional selectors by decreasing the switching time of selector feet comprised in the selector to less than the switching times of selector feet in conventional selectors.
When in operation, a selector foot constantly switches back and forth between selection positions at a rapid rate. When switching between selection positions, the selector foot generally moves a distance of about 2 mm in about 10 msecs. This change is resisted by friction, forces arising from part wear, machine design and tolerances, and random motional forces that occur during machine operation. The sum of these forces is on the order of between 0.2 and 0.5 Newton. Because of the close spacing within modem knitting machines and the small sizes of many of their components there is little room available for motors or actuators to provide the work required to accomplish the switching. An actuator or motor that can be used to improve the switching time of a selector foot in a selector must therefore be small, capable of switching direction rapidly and able to provide work at a greater rate than that available from motors or actuators in conventional selectors.
Piezoelectric motors can be produced that are small and powerful for their size and that can provide large accelerations of moveable elements in directions which can be reversed in time periods of microseconds. The switching time of a selector foot can be reduced to less than the switching times of selector feet in conventional selectors by using an appropriate piezoelectric motor to switch the selector foot between selection positions, in accordance with a preferred embodiment of the present invention. A selector foot, in accordance with a preferred embodiment of the present invention, is coupled to a piezoelectric motor that can displace a moveable element at a rate of about 400 mm/sec against a force opposing the motion which is on the order of from 0.2 to 0.5 Newton. Preferably, the selector foot comprises a friction coupling surface region suitable for friction coupling with the piezoelectric motor. Preferably, the selector foot is coupled to the piezoelectric motor by resiliently pressing a surface region of the piezoelectric motor, or an appropriate hard friction nub attached to the surface of the piezoelectric motor, to the friction coupling surface region of the selector foot. Preferably, the piezoelectric motor coupled to the selector foot is of a type described in U.S. Pat. No. 5,453,653, which is incorporated herein by reference. As a result, a selector foot in a selector, in accordance with a preferred embodiment of the present invention, can be switched between selection positions in a time on the order of 5 msec (2 mm/[400 mm/sec]=5 msec).
A selector, in accordance with a preferred embodiment of the present invention, comprises a multiplicity of activation feet, in accordance with a preferred embodiment of the present invention, operated in parallel. Preferably, the number of the multiplicity of selector feet is on the order of 10. With a switching time for the selector feet of 5 msec, in accordance with a preferred embodiment of the present invention, this results in a decision frequency for the selector in the range of 2000 Hz (the decision frequency=N/τ with N=10 and τ=5 msec).
There is therefore provided in accordance with a preferred embodiment of the present invention a selector for a knitting machine, which knitting machine comprises a plurality of latch needles and an activation station, such that when a latch needle of the plurality of latch needles is in the activation station, said selector determines whether said latch needle is activated or not activated, comprising: at least one selector foot selectively positionable to an activate or a deactivate selection position, wherein said selector foot has a friction coupling surface; and a piezoelectric motor coupled to said friction coupling surface of the at least one selector foot; wherein vibrations in said piezoelectric motor cause said at least one selector foot to switch between activate and deactivate selection positions. Preferably, the piezoelectric motor is coupled to the friction coupling surface by a resilient force which presses a contact surface of the piezoelectric motor to the friction coupling surface. Alternatively, the piezoelectric motor has a friction nub and the piezoelectric motor is coupled to the friction coupling surface by a resilient force which presses the friction nub to the friction coupling, surface.
In some preferred embodiments of the present invention the friction coupling surface is cylindrical. In other preferred embodiments of the present invention the friction coupling surface is planar.
In some preferred embodiments of the present invention vibrations in the piezoelectric motor cause the selector foot to switch between selection positions by rotating the selector foot through a given angle. Preferably, the vibrations in the piezoelectric motor rotate the selector foot through the given angle in a period of time less than 10 msec. More preferably, the vibrations in the piezoelectric motor rotate the selector foot through the given angle in a period of time less than 7 msec. Most preferably vibrations in the piezoelectric motor rotate the selector foot through the given angle in a period of time less than 5 msec. In some preferred embodiments of the present invention, the vibrations in the piezoelectric motor rotate the selector foot through the given angle in a period of time substantially equal to 5 msec.
In yet other preferred embodiments of the present invention vibrations in the piezoelectric motor cause the selector foot to switch between selection positions by causing a given linear displacement in the position of the selector foot. Preferably, the vibrations in the piezoelectric motor cause the given linear displacement in the position of the selector foot in a period of time less than 10 msec. More preferably, vibrations in the piezoelectric motor cause the given linear displacement in the position of the selector foot in a period of time less than 7 msec. Most preferably the vibrations in the piezoelectric motor cause the given linear displacement in the position of the selector foot in a period of time less than 5 msec. In some preferred embodiments of the present invention vibrations in the piezoelectric motor cause the given linear displacement in the position of the selector foot in a period of time substantially equal to 5 msec.
In some preferred embodiments of the present invention the at least one selector foot comprises a plurality of selector feet and each latch needle is associated with a particular one of the plurality of selector feet and when a latch needle is in the activation station the latch needle is activated or not activated according to the selection position of the particular selector foot of the plurality of selector feet with which the latch needle is associated. Preferably, each of the plurality of selector feet is coupled to a different piezoelectric motor.
There is further provided, in accordance with a preferred embodiment of the present invention, a method for switching a selector foot between an activate selection position and a deactivate selection position comprising: a) providing said selector foot with a friction coupling surface; b) coupling a piezoelectric motor to said friction coupling surface; and c) using vibrations of said piezoelectric motor to switch said selector foot between said activate selection position and said deactivate selection position. Preferably, coupling the piezoelectric motor to the friction coupling surface comprises pressing a contact surface of the piezoelectric motor to the friction coupling surface with a resilient force. Preferably, the piezoelectric motor has a friction nub and coupling the piezoelectric motor to the friction coupling surface comprises pressing the friction nub to the friction coupling surface with a resilient force.
Preferably, providing the selector foot with a friction coupling surface comprises forming a cylindrical friction surface. Alternatively, providing the selector foot with a friction coupling surface comprises forming a planar friction surface.
In some preferred embodiments of the present invention using vibrations of the piezoelectric motor to switch the selector foot between the activate selector position and the deactivate selector position, comprises using the vibrations to rotate the selector foot through a given angle. Preferably, using vibrations of the piezoelectric motor to switch the selector foot comprises using the vibrations to rotate the selector foot through the given angle in a period of time less than 10 msec. More preferably, using vibrations of the piezoelectric motor to switch the selector foot comprises using the vibrations to rotate the selector foot through the given angle in a period of time less than 7 msec. Most preferably, using vibrations of the piezoelectric motor to switch the selector foot comprises using the vibrations to rotate the selector foot through the given angle in a period of time less than 5 msec. In some preferred embodiments of the present invention using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to rotate the selector foot through the angle in a period of time substantially equal to 5 msec.
In other preferred embodiments of the present invention, using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to cause a given linear displacement in the position of the selector foot. Preferably, using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to cause the given linear displacement in a period of time less than 10 msec. More preferably, using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to cause the given linear displacement in a period of time less than 7 msec. Most preferably, using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to cause the given linear displacement in a period of time less than 5 msec. In some preferred embodiments of the present invention using vibrations of the piezoelectric motor to switch the selector foot, comprises using the vibrations to cause the given linear displacement in a period of time substantially equal to 5 msec.
BRIEF DESCRIPTION OF FIGURES
The invention will be more clearly understood by reference to the following description of a preferred embodiment thereof read in conjunction with the attached figures listed below, wherein identical structures, elements or parts which appear in more than one of the figures are labeled with the same numeral in all the figures in which they appear, and in which:
FIG. 1 shows a schematic of parts of a conventional selector used with a shuttle type activation station in a linear knitting machine having a needle bed;
FIGS. 2A-2C show details of the construction and operation of a conventional selector foot;
FIG. 3 shows schematically parts of a selector, in accordance with a preferred embodiment of the present invention for use with the same shuttle type activation station and linear knitting machine shown in FIG. 1; and
FIGS. 4A-4C show the details of construction and operation of a selector foot in accordance with a preferred embodiment of the present invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
FIG. 1 shows a schematic of parts of a conventional selector 20 used with a shuttle type activation station in a linear knitting machine having latch needles held in a needle bed. In this and in the other figures only those parts of the knitting machine, selector and latch needles are shown that are needed for understanding the operation of the selector shown in the figure. The knitting machine needle bed holds a plurality (typically thousands) of latch needles with shafts 22 formed with activation fins 24 in a closely packed parallel array in which the needles are equally spaced from each other. Activation fins 24 are staggered at different positions along the lengths of shafts 22 , and shafts 22 are positioned in the needle bed in such a manner, that activation fins 24 are accurately aligned in N parallel equally spaced rows perpendicular to shafts 22 . In FIG. 1A, N=10. The rows are indicated by dashed lines 25 and the first two activation fins 24 of each row are shown. Between any two consecutive activation fins 24 in a row of activation fins 24 there are N−1 latch needles, i.e., the distance between two consecutive activation fins 24 in a same row of activation fins 24 is N times the distance between adjacent latch needles.
Selector 20 comprises a selector frame (not shown) and an array of N selector feet 26 . Selector feet 26 are mounted in a row in the selector frame so that they are parallel to each other and equally spaced one from the other. Each selector foot 26 is mounted to the frame by means of a pin 28 around which selector foot 26 is rotatable. A bimorph activator 30 is coupled to each selector foot 26 by a U coupler 32 having arms 34 and 36 . The space between adjacent selector feet 26 is equal to the space between adjacent rows of activation fins 24 .
Selector 20 moves together with the shuttle activation station of the knitting machine as the activation station shuttles back and forth over the knitting machine's needle bed. Selector 20 moves over and parallel to the needle bed and in a direction parallel to the rows, i.e., parallel to lines 25 , of activation fins 24 , with each selector foot 26 maintained accurately aligned over and close to a different row of activation fins 24 . Each selector foot 26 therefore moves over latch needle shafts 22 in the needle bed along a different row of activation fins 24 and encounters an activation fin 24 once for every N needle shafts 22 that the selector foot 26 passes.
FIGS. 2A-2C show details of the construction and operation of a selector foot 26 . FIG. 2A shows a bimorph activator 30 coupled to selector foot 26 . Bimorph activator 30 is a long thin rectangular strip of piezoelectric material having large face surfaces 38 and ends 40 and 42 . End 40 is situated between arms 34 and 36 of a U connector 32 . End 42 of bimorph 30 is fastened to the frame (not shown) of selector 20 . Bimorph activator 30 bends when a potential difference is applied between faces 38 , otherwise bimorph 30 is straight. In FIG. 2A there is no potential difference between face surfaces 38 , and bimorph 30 is straight. When a potential difference is applied between face surfaces 38 , bimorph 30 bends into an arc shape with one of face surfaces 38 concave and the other convex. The direction of the bend depends upon the polarity of the applied potential. The bend causes end 40 to displace and, depending on the polarity of the applied potential, push against and apply a force to arm 34 or arm 36 of U coupler 32 .
FIG. 2B shows bimorph 30 when a potential difference is applied between face surfaces 38 that causes bimorph 30 to bend so that end 40 presses on arm 36 of U connector 32 . The pressure exerted by end 40 on arm 36 causes selector foot 26 to rotate clockwise through a small angle. FIG. 2C shows bimorph 30 when a potential difference is applied between face surfaces 38 which is opposite in polarity to the potential difference applied to face surfaces 38 in FIG. 2 B. In this case bimorph 30 bends in a direction opposite to the bend direction shown in FIG. 2B, and end 40 of bimorph 30 presses on arm 34 of U connector 32 . The pressure exerted by end 40 on arm 34 causes selector foot 26 to rotate counterclockwise through a small angle. The size of the angle through which selector foot 26 rotates when end 40 presses on one of arms 34 or 36 depends upon the amplitude of the voltage applied between face surfaces 38 .
In FIG. 2C, the potential difference applied between face surfaces 38 of bimorph 30 is sufficient to cause selector foot 26 to rotate clockwise by an angle large enough so that selector foot 26 is in a deactivate selection position. In this selection position, as selector 20 moves along rows of activation fins 24 , selector foot 26 will “collide” with and depress any activation fin 24 that it encounters. This will deactivate the needle to which the activation fin 24 is connected.
In FIG. 2B, on the other hand, a potential difference is applied between face surfaces 38 of bimorph 30 which has a polarity opposite to the potential difference applied to face surfaces 38 in FIG. 2 C and which is large enough to cause selector foot 26 to rotate clockwise into an activate selection position. In this position selector foot 26 is out of the way of onrushing activation fins and when it encounters an activation fin 22 , it will not collide with the activation fin 24 . It will “miss” and pass by the activation fin 24 and not depress it. The latch needle to which the activation fin 24 is connected will therefore be activated by the activation station.
FIG. 3 shows schematically parts of a selector 50 , in accordance with a preferred embodiment of the present invention, for use with the same shuttle type activation station and linear knitting machine with which the prior art system shown in FIG. 1 is used.
Selector 50 preferably comprises a selector frame (not shown) and an array of N selector feet 52 . N is preferably on the order of 10 (FIG. 3 is shown with N=10). Selector feet 52 are preferably mounted in a row in the selector frame so that selector feet 52 are preferably parallel to each other and equally spaced one from the other. Each selector foot 52 is mounted to the frame by means of a pin 54 around which selector foot 52 is rotatable. Selector foot 52 is preferably formed with, or mounted with, a friction coupling surface 56 . Friction coupling surface 56 is preferably a circularly cylindrical surface with axis congruent with the axis of pin 54 . Friction coupling surface 56 couples selector foot 52 to a piezoelectric motor 58 which is mounted to the selector frame by methods known in the art. The space between adjacent selector feet 52 is equal to the space between adjacent rows of activation fins 24 .
FIGS. 4A-4C show the details of construction and operation of a selector foot 52 . Referring to FIG. 4A, selector foot 52 is shown between activate and deactivate selection positions, in the same orientation with respect to the needle bed of the knitting machine as the orientation of selector foot 26 in FIG. 2 A.
Piezoelectric motor 58 is preferably formed in the shape of a thin rectangular plate having two large planar faces 60 , and short edge surfaces 62 and 64 . For exciting vibrations in the body of piezoelectric motor 58 one planar face surface 60 preferably has at least two surface electrodes and the other planar face surface 60 preferably has at least one surface electrode. Preferably, piezoelectric motor 58 has four quadrant surface electrodes 66 on one face surface 60 and a ground surface electrode on the other, hidden face surface 60 . Piezoelectric motor 58 preferably has a friction nub 68 fixed to edge surface 62 , for coupling to friction coupling surface 56 . Preferably, piezoelectric motor 58 is of the type described in U.S. Pat. No. 5,453,653.
Friction nub 68 is preferably pressed to friction coupling surface 56 by a resilient force 70 applied between short edge 64 and a frame (not shown)of selector 50 . Quadrant electrodes 66 and the ground electrode of piezoelectric motor 58 are preferably connected to a control circuit (not shown) which electrifies them to produce vibrations in the body of piezoelectric motor 58 as described in U.S. Pat. No. 5,453,653. The vibrations preferably produce clockwise or counterclockwise elliptical motion in friction nub 68 which produce respectively clockwise or counterclockwise frictional forces tangent to friction coupling surface 56 . These frictional forces produce torques which rotate selector foot 52 clockwise and counterclockwise to switch selector foot 52 respectively into a deactivate selection position or an activate selection position. FIG. 4B shows selector foot 52 in a clockwise, activate selection position, and FIG. 4C shows selector foot 52 in a counterclockwise, deactivate selection position.
Preferably, piezoelectric motor 58 can displace a moveable element at a rate of about 400 mm/sec against a force opposing the motion on the order of from 0.2 to 0.5 Newton. At this rate of displacement, assuming the radius of friction coupling surface 56 is 10 mm, piezoelectric motor 58 can rotate selector foot 52 at an angular velocity of about 40 radians/sec or about 2350°/sec. Assuming selector foot 52 must be rotated about 15° to switch selector foot 52 from a deactivate to an activate selection position, selector foot 52 can be switched between selection positions, according to a preferred embodiment of the present invention, in a switching time of about 5 msec.
A selector 50 , in accordance with a preferred embodiment of the present invention, having 10 selector feet 52 operating with a switching time of 5 msec operates at a decision frequency of 2000 Hz.
The present invention has been described using a non limiting detailed description of a preferred embodiment thereof. Variations of the embodiment described will occur to persons of the art. For example, a selector foot can be constructed so that instead of being rotated to switch between selection positions, the selector foot is displaced linearly to switch between selection positions. In this case a friction coupling surface of the selector foot would be a planar surface and selector feet would be mounted to a selector frame so that they slide along appropriate linear guides in the selector. It should also be realized that switching time is a function of the way in which the piezoelectric motor is coupled to the selector foot, the dimensions of the selector foot and the amplitude of the motion needed to switch the selector foot between selection positions. For the cylindrical friction coupling surface described above and a piezoelectric motor of constant speed (and variable power output), for example, switching time is proportional to the radius of the friction coupling surface. Additionally, while the detailed description of a preferred embodiment of the present invention refers to a selector used with a linear knitting machine, a selector in accordance with a preferred embodiment of the present invention, is similarly constructed for selecting latch needles in rotary knitting machines. | The present invention provides a method for rapidly switching selector feet ( 52 ) between activate and deactivate selection positions by friction coupling them to vibratory piezoelectric motors ( 58 ) and a fast selector ( 50 ) for a knitting machine comprising selector feet friction coupled to piezoelectric motors. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable.
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a structural method of arranging electronic packages within a standard electronics rack housing. More particularly, the present invention relates to a system of arranging electronic packages within an electronics rack so that rack space is used more efficiently and that rapid exchanges of the electronics packages is possible.
BACKGROUND OF THE INVENTION
The necessity for specialized computer equipment has increased dramatically over recent years. Corporations, both large and small, as well as individual consumers have come to depend on computers to enhance and assist them in a broad assortment of tasks. For the individual or small business, personal computers are typically relatively compact and streamlined, often comprising a monitor, a keyboard, a mouse, and a CPU “box” that sits on a desktop or on the floor. These personal computers, although considered compact when deployed in relatively small numbers, can be quite cumbersome and bulky when deployed in larger quantities. It is not uncommon for an organization to require several computers to act as servers controlling their local area networks. Even the networks of small companies run more efficiently when specific tasks are split up among individual servers. Typically, the small company will have a room with several servers, all in standard CPU cases consuming a significant amount of space.
For larger corporations that require numerous servers, the traditional CPU package is not practical to house servers. Larger companies, especially “e-businesses” that use the internet and the world wide web to conduct their commerce, require a higher number of servers than that required by smaller businesses. Such organizations, and in particular the internet service providers, or ISPs, must be able to pack far more server appliances within a limited amount of space than would be conceivable using traditional desktop chassises. For such operations, an industry standard EIA (Electronics Industries Alliance) rack is often used to contain servers in a stacked arrangement that uses the available space more efficiently.
Such electronics racks are a relatively simple structure that closely resemble an open-frame bookcase without shelves. Computer server/component racks are typically constructed with perforated, hinged front-doors, rigid sides and a removable rear panel. Often, the rear panel of an electronics rack is constructed as a hinged, perforated door that is allowed to be opened and swung out of the way when access from the rear is desired. Within the rack exterior, or “shell,” formed by the sides and back panel is a structural frame. The rack frame is capable of supporting the weight of the electronics contained within the rack and serves as the primary means of securing components therein. The rack frame, closely resembles an industrial shelving unit and typically includes four rigid corner posts, connected to each other with a plurality of cross members and structural supports. Each of the four comer posts include a plurality of mounting holes, though which electronic components can be secured.
Industry standard 19″ EIA electronics racks are designed typically to house a column of electronics packages that are 17 ¾″ in width and with varying depths. The height of an electronics package can vary but, to be compatable with the rack mounting structure, must be an integer multiple of an EIA unit called simply the “U.” An EIA U is 1.75 inches. Electronic equipment generally has a height in multiples of “U's” e.g., 1U (1.75″), 2U (3.50″), 3U (5.25″), etc. A piece of equipment whose height is not an integer multiple of a U will not efficiently use rack space. Standard equipment racks are available in a wide assortment of heights, but the most common is of 42U height.
Typically, electronic packages are mounted in the rack from the front and secured in place with fasteners, specifically thumbscrews. The thumbscrews allow frequent installation and removal of the electronic packages with minimal effort and without hand tools. Power and data connections are preferably made by opening the rear panel of the rack and accessing the rear surface of the mounted device. If a piece of equipment is heavy or does not include features that allow it to be secured properly to the rack, a rack shelf can be secured in place to the rack frame to support the non-standard device. Alternatively, electronic components may be secured within the rack using a pair of drawer slides. The drawer slides, usually ball-bearing supported rails, are secured in place within the rack frame. Corresponding rails are located on the side surfaces of the electronics component to be mounted, thus allowing the component to be pulled in and out of the rack frame easily to allow quick and frequent access.
Although it is preferred that the height of the electronics components be a multiple of the standard EIA unit U, the dimension of the EIA unit is understood to represent a maximum allowable height. Two adjacent 1U height electronic devices will require a finite amount of clearance. This amount of clearance aides in the installation of the rack mounted electronics and promotes interference free insertion and removal. For a device that is much less heat intensive, for example an internet server, an overall height of 1.65″ (with 0.05″ clearance above and below) can be used for a 1-U package. In either example, a few thousandths of an inch of clearance room must be vacated to enable ease of installation.
A piece of electronics equipment that is mounted in a chassis may vertically span more than one EIA unit of height. For example, a power supply module could be mounted into an EIA rack system and allotted a vertical space equivalent to 4Us (1.75″×4=7″). If the manufacturer desires a minimum vertical clearance allowance (top and bottom) of 0.100 inches for example, the power supply could then be constructed to be 6.800 inches [(7.000−(2×0.010)] in height without concern for interfering with the installation or operation of adjacent pieces of equipment.
Of course, it is always desirable to make electronic equipment smaller. Smaller electronic equipment means that more pieces of equipment can be housed in a rack. Unfortunately, as the desire for miniaturization of electronics devices progresses, the standard minimum vertical amount of rack space, 1-U, has remained substantially unchanged. Since the U represents a minimum height, a piece of equipment that has a height that is less than 1.75″ must still be mounted so as to take up a full U of height. To compensate for the required height, compact equipment often will not extend to the full depth (15″ vs. 30″, for example) of the rack. When components that do not extend the full depth are mounted in a standard rack, space can be wasted and an important benefit of the rack mounting of components is diminished. While it would be possible to design a new rack system with a new set of standards for equipment size, it is preferable to create a means to modify the storage capabilities of current EIA racks to allow more storage configurations to be achievable within the confines of a standard “legacy” rack. Many companies have already invested significant amounts of money on their current facilities and equipment and would prefer not to have to change their equipment. Furthermore, it is not entirely practical to arrange systems to occupy less than a full EIA unit of height as devices that are often accessed at the front of a rack-mounted package (e.g., disk drives) require more height than such an arrangement would allow.
In an attempt to conserve rack space, some have mounted two half-depth, 1-U systems in a rack, one from the front and another from the back of a 1-U space, in a “back-to-back” configuration with limited success. Although this method allows two devices to be secured within a single space, much of the functionality and benefit of the rack design is lost. For instance, because the systems are mounted “back-to-back,” the cabling that is required to power and communicate with the equipment located toward the back of the rack is now located in the center of the rack, in a location generally inaccessible without removing at least one electronic package. Further, these cables must be redirected either through a side or the middle of the rack in a manner that is completely unserviceable to a system administrator without disabling some of the affected components.
Because EIA racks are so widely deployed and already represent a highly efficient means to package and store electronic components, a method to store more equipment within the confines of an existing EIA rack is highly desirable. Currently, there is no known way to conveniently house two, three, or more distinct electronic packages within a 1-U EIA rackspace from the front and trends in server appliance miniaturization and redundancy are increasingly demanding such a feature. The ease of installation, removal, replacement, and interchangeability would be greatly improved with a system that could efficiently pack such equipment.
BRIEF SUMMARY OF THE INVENTION
The present invention overcomes the deficiencies of the prior art by providing a system to mount several servers within a 1-U space of a standard EIA electronics rack. The system includes a mounting tray, or chassis, that is securely fastened to a standard 19″ EIA electronics rack. The tray includes dividers that define at least two full length ports per EIA unit into which electronic packages are slidably engaged. Furthermore, each port defined by the mounting tray includes hot-pluggable blind-mate sockets to receive corresponding hot-pluggable blind-mate connectors upon each electronics package. These packages are engaged and disengaged to and from the ports within the rack at will, thus allowing for more servers to be efficiently and accessibly stored within the confines of a 1-U rackspace than was previously possible.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more detailed description of the preferred embodiment of the present invention, reference will now be made to the accompanying drawings, wherein:
FIG. 1 a perspective view drawing of an interchangeable server mount system in accordance with a preferred embodiment of the present invention;
FIG. 2 is a perspective view drawing of an electronic package in accordance with a preferred embodiment, of the present invention that is to be contained within the server mount system of FIG. 1; and
FIG. 3 is a rear view perspective view drawing of the electronic package of FIG. 2 .
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to FIG. 1, an interchangeable electronics rack mount system 100 is shown. Interchangeable rack mount system includes a mounting chassis 102 positioned preferably within a 1U rackspace of a standard 19″ EIA rack assembly 104 . Mounting chassis 102 preferably spans the width of the rack assembly 104 . A standard 1U space of EIA standard 19″ rack 104 is 1.75 inches of height, 17 ¾ inches of usable width, and a varying degree of depth (preferably 30 inches). Mounting chassis 102 is positioned horizontally within rack 104 and secured in place by captive thumbscrews 106 . Rack 104 includes a plurality of vertically spaced mounting apertures 108 that receive screws 106 .
Mounting chassis 102 preferably includes a bottom 110 , a left and right side 112 , 114 , and a rear wall 116 . At least one divider 118 is mounted to the chassis bottom 110 and runs from the front of chassis 102 to the rear wall 116 . The divider 118 divides the chassis into multiple docking parts 120 . One divider 118 results in two docking parts. Two dividers create three docketing parts, and so on. Divider 118 is positioned substantially parallel to sides 112 and 114 . By placing dividers 118 at various positions within chassis 102 parallel to sides 112 , 114 , different sized docking ports 120 can be created. Although it is preferable for each chassis 102 to contain 2 or 3 equally sized docking ports 120 , it should be understood that the relative size and number of ports 120 within chassis 102 can be any number desired. Preferably, located within the front left side of each port 120 , is a latch recess 128 . Recess 128 can take the form of a simple cutout in a divider 118 or in the left or right side 112 , 114 of chassis 102 . At the rear of each port 120 of chassis 102 is a docking bulkhead 122 that receives power and data connections of a piece of equipment inserted into docking port 120 . Referring still to FIG. 1, bulkhead 122 preferably includes sockets that mate with corresponding blind-mate connectors on the piece of equipment in docking port 120 . Although a variety of sockets can be used, preferably at least one power socket 124 and at least one communications socket 126 are included in the docking bulkhead 122 .
Referring now to FIG. 2, an electronics package 150 is shown disposed within a docking port 120 . The electronics package can be any type of digital or analog device such as a server, a storage system, or a power supply. Electronics package 150 is preferably constructed with a housing 152 and a front panel 154 . Front panel 154 preferably includes a handle 156 and a latch 158 for securing package 150 in position within mounting chassis 102 . Although not shown in FIG. 2, front panel 154 can include accessible floppy and CD-ROM drives to allow a user to upload and download data and configuration settings to a computing device contained within package 150 .
Referring now to FIG. 3, the rear surface of electronics package 150 is shown as having a rear panel 160 with power and communications hot-pluggable blind mate connections 162 and 164 which mate with the power and communications sockets 124 , 126 of bulkhead 122 of FIG. 1 . As blind mating hot-pluggable connectors, connectors 162 , 164 automatically connect to corresponding bulkhead sockets 124 , 126 when the electronics package 150 is fully inserted into docking port 120 .
Referring to FIGS. 1-3 together, electronics rack mount system 100 is installed by first installing chassis 102 into rack 104 and securing with thumbscrews 106 . Chassis 102 is constructed to fit within the limitations of 1-U of EIA rackspace and multiple chassis 102 can be installed within vertically adjacent rack spaces together to form an array of ports 120 . For example, five chassises 102 , each with 3 ports 120 , could be stacked on top of each other in a rack to form an array of 15 docking ports 120 . Alternatively, a single chassis can be constructed to span vertically across more than one EIA unit and thus hold an array of ports 120 . For example, the 15-port array mentioned above could be created by installing a single 5-U chassis with each “U” containing 3 docking ports 120 . A potential advantage of such an arrangement could include the ability to share a common power or data distribution system across the entire array. For example, one power cable could be used to supply power to each of the power sockets in the array, thus eliminating a significant amount of cable clutter at the rear of rack 104 .
Once chassis 102 is secured within rack 104 , connections at the rear of rack 104 are made to connect the sockets of each port 120 to power and communications cables. With the chassis 102 installed and connected, the server mount system 100 is ready for operation. Electronics packages 150 are slidably engaged into ports 120 created by dividers 118 and side rails 112 , 114 . Packages 150 are slid into the ports 120 until they contact against rear wall 116 of chassis. As electronics packages 150 contact against rear wall 116 , blind-mate hot-pluggable connectors 162 , 164 of rear panel 160 mate with bulkhead socket connectors 124 , 126 . Power socket 126 of bulkhead 122 mates with power receptacle 162 of package 150 and communications socket 124 mates with connector 164 . When fully engaged into aport 120 , spring-loaded latch 158 of electronics package 150 engages recess 128 within chassis 102 , thus preventing removal of packages from server mount system 100 . When removal of package 150 is desired, the user slides latch 158 away from recess 128 and can then remove package 150 by grasping handle 156 and pulling package 150 away from port 120 . Furthermore, a latch activated electronic sensor (not shown) may be included within latches 158 to notify a system to prepare itself for its removal from a port 120 .
Electronics mount system 100 offers the user the ability to replace servers, or any other electronic device, quickly and with little effort. Furthermore, the electronics mount system 100 of the present invention represents a dramatic improvement to the device capacity of a standard EIA rack. With conventional designs, it was only practical to store one component within a 1-U unit of rackspace. Alternative methods for housing several components within a single rackspace eliminated much of the functionality and convenience that is associated with the EIA rack mount design. A system in accordance with the preferred embodiment of the present invention allows the installation of multiple, full length packages within a single standard 1-U rackspace. By increasing the number of packages (from 1 per EIA unit to 2 or 3) rack users that require a high number of servers, or any other rack mounted components, can store them more efficiently. This more efficient use of the storage space within an EIA rack allows businesses to expand their computing power and customer base without need for more office space.
In deploying a system in accordance with the preferred embodiment of the present invention, EIA Rack users can store multiple appliances within a single rack space without departing from the features and spirit of the EIA rack mount concept. Such features include, but are not limited to, ease of installation into and removal from the rack, front panel access and input to the system, and connection access to the rear of the system.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that the drawings and detailed description thereto are not intended to limit the invention to the particular form disclosed, but on the contrary, the intention is to cover all modifications, equivalents and alternatives falling within the spirit and scope of the present invention as defined by the appended claims. | A system to mount several electronic devices within a one EIA unit high rackspace is presented. The system includes a mounting chassis that is securely fastened to a standard 19″ EIA electronics rack. The chassis includes dividers that define at least two full length ports in which the electronic devices are slidably engaged. Furthermore, each port defined by the mounting tray includes hot-pluggable, blind-mate sockets to receive corresponding hot-pluggable, blind-mate connectors upon each electronics package. These packages are engaged and disengaged to and from the ports within the rack at will, thus allowing for more servers to be efficiently and accessibly stored within the confines of a 1-U rackspace with interchangeability than was previously possible. | 7 |
This Non-Provisional Application is based on and claims the Priority of previously filed Provisional Applications 61/324,302 filed on Apr. 15, 2010. The disclosures made in Applications 61/324,302 are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates generally to systems and methods of network-based communication systems. More particularly, this invention relates to the systems and methods of techniques for information content management in the network-based communication systems.
2. Description of the Related Art
Even though there are tremendous progresses made in the data and media content generation, storage, search, transmission and presentation technologies, there are still difficulties and limitations for a network user to convenient perform an enquiry and search process. Specifically, the process of entering the “enquiries” to start a search process often requires a wireless network user to interact with a search system in multiple “refining search” steps by repeating a user's “key-in” enquiry entry step followed by a the search system's response with a “search result presentation” step. Such step-by-step interactively and progressively refining search processes often require a user to type on a miniaturized device with a very small keypad. The search processes become very inconvenient and difficult for these mobile device users.
Such difficulties and limitations cannot be easily resolved due to the basic reasons that the framework of “enquiry entry” and “search” process are often built-in as part of the “operating system” of a mobile devices and the search systems. Changes of the search processes require fundamental and complicate changes to the software supported by the device and also by the search engine called by the mobile devices.
In the meantime, one of the most rapidly expanding aspects of wireless networking involves the accessing of information content over wireless networks via web-enabled mobile devices. Examples of such devices include mobile telephones, personal digital assistants (PDAs), palmtop computers, etc. As is well-known, these and other web-enabled devices not only provide access to the Internet, but can also be used to support other types of wireless networking functionality, such as messaging, distributed collaboration, and location-based services. With the expanded applications of wireless networked devices, especially the increased number of mobile devices, an urgent need exists to resolve the limitation and inconveniences caused by the requirement to key in multiple levels of enquiries before the proper and most relevant search results can be assessed.
Therefore, a need still exists in the field of wireless web-based network communication to provide new and improved system configuration and methods to overcome such limitations.
SUMMARY OF THE PRESENT INVENTION
It is therefore an aspect of the present invention to provide new and improved system configuration and methods to for information and content management in the networked-based communication systems to build a “5W1H” like equerry process. The “5W1H” like equerry process is built on top of the traditional operation system by applying an inter-application or inter-process link scheme without requiring changes made to the operation system of a device or a server such that the “5W1H” like equerry process can be conveniently implemented as a filter to significantly enhance the search/enquiry processes.
Another aspect of the present invention is to provide new and improved system configuration and methods to for information and content management in the networked-based communication systems to build a “5W1H” like equerry process to simplify the operations and processes of the mobile device users. The present invention can provide simplify and convenient processes for a user to easily build a data-space or to enter into a user-targeted cyber space. The present invention can therefore eliminate substantially all of the efforts to search first followed by browsing many retrieved links to select for entering the most relevant cyber space as that often required in the convention processes. The user can quickly and conveniently achieve a more targeted enquiry and accurate retrieval to recognize, watch, communicate, or engage other networked based interactions as intended by the user.
Briefly, in an embodiment, the present invention discloses an apparatus for use in managing information content in a network-based communication system. The apparatus comprising a processing element comprising a processor coupled to a memory. The processing element provides at least a portion of a content management web site identified by a first uniform resource locator and accessible to a user of the communication system, the content management web site permitting the user to enter a plurality of defining terms as search filters for searching and retrieving uniform resource locators for linking to contents relevant to the defining terms entered by the user. In an embodiment, the content management web site constituting a first application calls second applications to permit the user to enter the plurality of defining terms as search filters for searching and retrieving uniform resource locators for linking to contents relevant to the defining terms entered by the user.
In another embodiment, this invention discloses a mobile communication device operated with an operating system to control and manage a plurality of application processes. The mobile communication device further includes a 5W1H, i.e., who-what-when-where-why and how application, called by at least one of the application processes to allow a user of the mobile communication device to enter 5W1H scope-definition terms to carry out the application calls the 5W1H application.
These and other objects and advantages of the present invention will no doubt become obvious to those of ordinary skill in the art after having read the following detailed description of the preferred embodiment, which is illustrated in the various drawing figures.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a system functional diagram for showing a network-based communication system configured in accordance with an illustrative embodiment of the invention.
FIG. 2 is system diagram for showing data transmission and processes among the network-based communication system to carry out the user enquiry and retrieval among a mobile device and/or servers of the present invention.
FIG. 3 is a flowchart to illustrate the processing steps carried among the mobile devices and the operating system of a base station or a server to enable the “5W1H” search according to user defined scope of this invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
FIG. 1 is a system functional diagram for showing a network-based communication system 100 configured in accordance with an illustrative embodiment of this invention. The system 100 includes a wireless network 105 coupled to the Internet 110 , a set of mobile devices 115 , a set of servers 120 and a set of user terminals 125 . As shown in FIG. 1 , the numbers n, k, and r are adjustable integer numbers to denote the n mobile devices 115 - 1 , . . . 115 - n are coupled to the wireless network 105 , k servers 120 - 1 , . . . 120 - k and r user terminals 120 - 1 , . . . 120 - r are coupled to the Internet 110 . Also, alternative embodiments of the invention may not include the particular system elements shown, and may include other elements of a type and configuration known to those skilled in the art, in place of or in addition to the particular elements shown. The mobile devices 115 and user terminals 125 may be more generally referred to herein as user devices. The term “user” is intended to include, without limitation, an individual, a group of individuals, a business, an organization, or any other entity capable of deriving benefit from use of at least a portion of the system 100 . Actions described herein as being performed by or otherwise associated with a user may be performed by or otherwise associated with an individual or other entity, a corresponding device, or both the entity and the device. The network configuration of system 100 is shown only as an example. The present invention is not limited by the configuration as shown. The Internet as shown may include an intranet, an extranet, a wide area network (WAN), a metropolitan area network (MAN), a wired local area network (LAN), an IEEE 802.11 or Wi-Fi wireless LAN, a satellite communications network, a virtual private network (VPN), a public switched telephone network (PSTN), a cellular network based on third generation (3G) wideband code division multiple access (CDMA) or other standard, as well as portions or combinations of these and other networks.
The mobile devices 115 may collectively comprise a wide variety of different devices configurable for communication over the network 12 . The term “mobile device” as used herein is intended to include, without limitation, any type of portable information processing device capable of being configured for communication over a network. Examples of mobile devices 115 utilizable in FIG. 1 include a mobile telephone, a personal digital assistant (PDA), a palmtop computer, a hand-held computer, a laptop computer, a tablet computer, a global positioning system (GPS) receiver or other GPS-based navigational device, an MP3 player or other type of audio player, a pager, a watch or other timepiece, a camera, a portable game player, etc. The servers 120 may comprise, by way of example, network computers or other types of computers or processing elements capable of being configured for the maintenance, storage, delivery or other processing of information received or deliverable over the Internet or other type of network. Furthermore, one or more of the user terminals 120 may each comprise a mobile device. Also, a given one of the user terminals 120 may comprise a non-mobile device, including, by way of example, a desktop personal computer, a workstation, a minicomputer, a mainframe computer, a television, a set-top box, a kiosk, etc.
As commonly understood that each of these mobile devices, servers, user terminals, can function as an independent data processing element and each of these data processing elements may include a process, a memory for data storage and a network or communication interface to connect to a network based communication system either through physical connections or through wireless interconnections.
FIG. 2 is a system functional diagram and FIG. 3 is a flowchart to illustrate the processes performed in a mobile device by applying an inter-application communication scheme to build a “5W1H” like system of this invention. It is understood that such processes may be carried among a user and a server or a user terminal as well as that shown in FIG. 1 . The inter-application communication process starts with a user starts an application (APP- 1 ) from a mobile device (Step 200 ). The APP- 1 then calls a 5W1H Application (APP- 2 ) of this invention to allow a user of the mobile device to enter and define scopes of enquiries that may include 5W1H filtering terms to start the online search process (Step 210 ). Then, the APP- 2 receives the user entry. The user entry may be in a form such as 5W1H://when&where&what/From=APP- 1 . The 5W1H Application then processes the user entries to determine if an inter-application system call is necessary depending on the scopes of data searches requested by the user (Step 220 ). If it is determined that a system call is not necessary, then an API return is provided to the APP- 1 . If the system call is necessary, then an inter-application communication call is made to the operation system (OS) of the mobile device, or a server depending on the scopes of the user request (Step 230 ). The processes are completed by retrieving a system API return from the OS back to the user through APP- 1 as the “result return” as that request by the user.
The scopes of the enquiries can be conveniently defined without requiring changes made to the operating systems of a mobile device or a server or any data processing element. The inter-application communication scheme can be applied to link different levels of application to conveniently and flexibly link and activate different applications to process and retrieve required data and content needed for different levels of “Applications” implemented in a mobile device or any of the data processing elements as shown in FIG. 1 .
Specifically, the 5W1H application, APP- 2 of this invention enable a user to enter different types of enquiry terms and to more completely and accurately define a scopes as a targeted enquiry to starts a search process. Such processes provide convenient and flexible applications for a mobile device user such that the typing and data entry requirements are greatly reduced. A user may define different types of scopes that may be distinctly targeted by using the following 5W1H like attributes for searching the media files available on the networks.
When:
Event_time, when the event happens;
Create_time, when the file created;
Upload time, when the file uploaded to the system;
Public time, when the file is public to all users (a file is private by default).
The time logic is Event_time<=Create_time<=Upload_time<=Public_time.
Where:
Event_Longitude/Event_Latitude, where the event happen;
Event_GPS_Accuracy (0-100%), it may be 0 if the data is not from real time GPS receiver;
Create_Longitude/Create_Latitude, where the file create;
Create_GPS_Accuracy (0-100%);
IP_range, what kinds of ip address.
In some cases such as movies, the Event and Create attributes are different; but for real time news video, they are same.
Who:
Leading roles(s), it may be the name(s) of one or plural person, pet or building etc;
Owner, the writer or photographer.
What:
Category, the content category, for example, it may be Drama for movie file; Rate, the content rated level, for example, PG for movie file.
Why:
reason, for_share or for_sale. And other attributes (metadata tag) mentioned in another patent application: APT 61/296,479 “Method and system for image/audio/video metadata”.
The following attributes will be defined for Applications:
When:
Start_time/End_time, the valid period for the application; Schedule_day/Schedule_hour, the valid schedule time to run the application.
Where:
Longitude/Latitude scope, the valid district for the application;
Who:
Exec_by, who can run the application, System, Owner or Guest.
What:
Category, the application type, for example, Game or Education; Rate, rated level.
Why:
Reason, for_share or for_sale.
How:
Real_time, if it runs all time even in background. 1. The Advertisement is a special Category application which will be executed by system only. The Advertisement developer must following the dedicated API to write the program and system will run it if some applications call the system advertisement function. 2. One or plural dSpace(s) can be defined in a system which can be a local computer system, network systems, or web-based system. Each dSpace will consist one or plural above media file(s) or application(s); 3. A dSpace is defined by series filter combinations with above file or application attributes and some special operators including BEFORE, AFTER, BETWEEN, IN, OUT, AND, OR and NOT etc. For example, the 2010 Winter Olympics dSpace will be defined as following filters: (between Feb. 12, 2010 and Feb. 28, 2010) and (Vancouver or Whistler) (by Longitude/Latitude scope) and (NOT Advertisement application)
So when the user entry this dSpace, only those media files match the above filters are available.
4. A dSpace can be private or public. For public dSpace, everyone can see and join the dSpace; For private dSpace, only invited users can see the dSpace end can be approved then join the dSpace. 5. The dSpace support guest members which can view the content or activities in the dSpace but they can't run the application(s) in the dSpace and participate the activities. 6. A friend dSpace concept is supported which means that the members of a friend dSpace are guest of the dSpace. 7. The dSpace support inheritance concept so the sub-dSpace will have the base dSpace filters. The inheritance support multiple inheritances which allow plural parents (bases) dSpaces. 8. The present invention support multiple dSpace login at the same time and the user can have a dedicated nickname for each dSpace. 9. There is a “real_time” attribute to define if a dSpace will still run when it's in background. The system will check all the background dSpaces and run those “real_time” applications inside the “real_time” dSpace only. 10. An IP_Range is defined for a dSpace to filter login user ip address. 11. A User_network_speed for a dSpace to filter login user connecting speed. 12. A dedicated dSpace API is provided for developer so that they can develop the application running inside dSpace and those dSpace, files, user attributes can be accessed.
Although the present invention has been described in terms of the presently preferred embodiment, it is to be understood that such disclosure is not to be interpreted as limiting. Various alternations and modifications will no doubt become apparent to those skilled in the art after reading the above disclosure. Accordingly, it is intended that the appended claims be interpreted as covering all alternations and modifications as fall within the true spirit and scope of the invention. Those approaches and mechanisms in the art will appreciate variations of the above-described embodiments that fall within the scope of the invention. As a result, the invention is not limited to the specific examples and illustrations discussed above, but only the following claims and their equivalents. | An apparatus for use in managing information content in a network-based communication system. The apparatus includes a processing element that includes a processor managed and operated by an operation system (OS) software and coupled to a memory. The processing element executes a first application to call a second application for permitting the user to enter a plurality of defining terms for the second application to apply the defining terms as search filters for searching and retrieving uniform resource locators for linking to contents relevant to the defining terms entered by the user. The second application further determines whether to call the OS depending on the search filters generated from the defining terms. | 6 |
This is a divisional application of application Ser. No. 08/611,867 filed on Mar. 6, 1996.
BACKGROUND OF THE INVENTION
In the course of treating and preparing subterranean wells for production, a well packer is run into the well on a work string or a production tubing. The purpose of the packer is to support production tubing and other completion equipment, such as a screen adjacent to a producing formation, and to seal the annulus between the outside of the production tubing and the inside of the well casing to block movement of fluids through the annulus past the packer location. The packer is provided with anchor slips having opposed camming surfaces which cooperate with complementary opposed wedging surfaces, whereby the anchor slips are radially extendible into gripping engagement against the well casing bore in response to relative axial movement of the wedging surfaces.
The packer also carries annular seal elements which are expandable radially into sealing engagement against the bore of the well casing in response to axial compression forces. Longitudinal movement of the packer components which set the anchor slips and the sealing elements may be produced either hydraulically or mechanically.
After the packer has been set and sealed against the well casing bore, it should maintain sealing engagement upon removal of the hydraulic or mechanical setting force. Moreover, it is essential that the packer remain locked in its set and sealed configuration while withstanding hydraulic pressures applied externally or internally from the formation and/or manipulation of the tubing string and service tools without unsetting the packer or interrupting the seal. This is made more difficult in deep wells in which the packer and its components are subjected to high downhole temperatures, for example, as high as 600 degrees F., and high downhole pressures, for example, 5,000 pounds per square inch ("psi"). Moreover, the packer should be able to withstand variation of externally applied hydraulic pressures at levels up to as much as 15,000 psi in both directions, and still be retrievable after exposure for long periods, for example, from 10 to 15 years or more. After such long periods of extended service under extreme pressure and temperature conditions, it is desirable that the packer be retrievable from the well, with the anchor slips and seal elements being retracted sufficiently to avoid seizure against well bore restrictions that are smaller than the retracted seal assembly, for example, at a makeup union, collar union, nipple or the like.
Currently, permanent packers are used for long-term placement in wells requiring the packer to withstand pressures as high as 15,000 psi at 600° F. Conventional permanent packers are designed in such a way that they become permanently fixed to the casing wall and that helps in the sealing of the element package. However, permanent packers must be milled for removal. One of the major problems involved in removing a permanent packer is that its element package normally has large metal backup rings or shoes that bridge the gap between the packer and the casing and provide a support structure for the seal element to keep it from extruding out into the annulus. The problem with that arrangement is that the large metal backup shoes act like a set of slips and will not release from the casing wall.
Present retrievable high pressure packers use multiple C-ring backup shoes that are difficult to retract when attempting to retrieve the packer. A further limitation on the use of high pressure retrievable packers of conventional design, for example, single slip packers, is that if there is any slack in setting of the packer, or any subsequent movement of the packer, some of the compression force on the element package is relieved. This reduces the total compression force exerted on the seal elements between the mandrel and the casing, therefore permitting a leakage passage to develop across the seal package.
Further, it is common knowledge in designing currently used retrievable high pressure packers that a longer slip can be used to more evenly distribute the load into the casing. However, what generally occurs is that a slip will reach a length with a corresponding length of slip tooth contact, such that it becomes difficult or impossible to achieve initial slip tooth penetration into the casing wall when setting the packer. There becomes so much tooth length in contact with the casing that the setting slip load is insufficient to anchor the packer.
Another problem in high temperaure, high pressure packers of any type involves the slips damaging the casing. With the axial loads and pressure differential loads at the design limits, the total axial force on the packer slip is almost 500,000 pounds. Discounting friction, this load is multiplied to a radial force into the casing wall when divided by the tangent of the slip/wedge contact angle. Since the packer may be set inside uncemented casing, potential casing damage is a major concern.
With conventional segmented slips, the inherent three- or four-point loading of the casing wall will deform the casing into a predisposed slip pattern, and the fully loaded unsupported casing will deform into roughly a triangle or a square, etc., corresponding to the number of individual slips used. Nodes will appear on the casing outer diameter corresponding to each slip segment. This result is not desirable, as it will then become very difficult to land and properly set another packer after the first one is removed. Further, as the tubing in such wells is typcially made of an expensive corrosion resistant alloy, scratches and indentations are to be avoided, as they can act as stress risers or corrosion points.
Therefore, what is needed is a packer capable of safely deploying at its design limits in totally unsupported casing, without damaging the casing.
Another problem with high pressure retrievable packers is that they cannot withstand high tubing loads during production and stimulation operations.
Another problem with high pressure retrievable packers is that no matter how well designed, they can sometimes accidentally release.
Therefore, it is an object of the invention to provide a retrievable packer that can operate efficiently at pressure differentials of 15,000 psi and temperatures to 600° F. without releasing.
It is further an object of this invention to provide a retrievable packer that has a slip design that allows longer slips to be effectively used.
It is further an object of this invention to provide a tighter element seal and a more dependable sealing system.
It is further an object of this invention to provide a retrievable packer that cannot be accidentally released.
SUMMARY OF THE INVENTION
The foregoing objects are achieved according to the present invention by a well packer having a barrel slip that is progressive set, which further includes a cinch slip to prevent accidental release. The barrel slip has cones that are generally complementary to cones on wedges that set the barrel slip, wherein the wedge cones are spaced so as to be progressively further distances apart from their complementary slip cones. Ordinarily, the mating wedges which deploy the slip would be machined in a like manner with matching diameters and distances between cones. However, in the inventive device, the gaps between the wedge cones and slip cones are progressively larger, as viewed from the center of the longitudinal center of the slip to its outer edges, wherein the section of slip where the angle of the wedges reverse is referred to as the center of the slip. Thereby, the cones of the wedges which mate with the centermost cones of the slip make contact first by design. This forces the center of the slip to be loaded first. The remaining wedge cones have not yet made contact with their complementary slip cones. As greater forces are exerted on the wedges from end to end, the wedge will deform slightly and the next cone of the wedge will make contact with its matching portion of slip. Continuing in a likewise manner, as the wedges are loaded higher and higher, more wedge cones come into bearing contact with the slip. The standoff between the cones of the wedges is controlled very precisely such that slight elastic yielding takes place by deforming the wedge inwardly.
This design effectively allows initial setting of the packer with very little slip tooth contact area. This permits the slip to quickly get a good grip into the casing wall. Subsequent higher loading brings more and more slip teeth to bear and prevents overstressing the casing. This design may also be used with a plurality of individual slips in place of the barrel slip.
Further, the use of a barrel slip provides full circumferential contact with the casing. This design effectively spreads the slip-to-casing load over a large area and minimizes slip-to-casing contact stresses. With the barrel slip, the casing is always urged into a circular cross section, even at full loads. Furthermore, the slip is designed to load uniformly such that equal loads are borne by all the slip teeth. This ensures minimum slip tooth penetration into the casing wall.
In another aspect of the invention, an internal cinch slip is used to retain the packer in its set position. The cinch slip is designed similarly to the barrel slip, and is flexible enough to easily ratchet over the mating bottom sub connector threads. It is spring loaded with simple wave springs, and eliminates "backlash" usually associated with a one piece heavy-duty cinch slip. Elimination of backlash creates a tighter element seal and provides a more dependable sealing system. The cinch slip serves to keep the packer in its set position and thereby prevent the accidental release of the packer.
In yet another aspect of the invention, the packer is purpose-designed as a cut-to-release packer. That is, this retrievable packer has no built-in release mechanism, but instead has a locking assembly that locks the packer in its deployed position. The only way it can be released is by severing the mandrel. In a preferred embodiment, a no-go shoulder is provided in the mandrel on which to positively locate a wireline chemical cutter. The cut point is thereby opportunely designed so that the mandrel is severed in a precise location such that not only is the packer released, but all the packer and tail pipe are then retrieved as a unit. No part of the packer is left in the well for subsequent fishing operations, nor is any milling required, as would be with a traditional permanent packer.
The primary advantage of a cut-to-release packer is that it can withstand extreme tubing loads occurring during production and stimulation. It also positively prevents accidental release of the packer.
The novel features of the invention are set forth with particularity in the claims. The invention will best be understood from the following description when read in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a longitudinal view in elevation and section of a retrievable well packer embodying the features of the present invention set in the casing of a well bore providing a releasable seal with the casing wall and a tubing string extending to the packer;
FIGS. 2A-2C, inclusive and taken together, form a longitudinal view in section of the retrievable well packer and seal assembly of the invention showing the seal assembly relaxed and the packer slips retracted as the packer is run into a well bore;
FIGS. 3A-3C, inclusive and taken together, form a longitudinal view in section of the retrievable well packer and seal assembly of the invention showing the seal assembly and the packer slips deployed as the packer is set in a well bore;
FIGS. 4A-4C, inclusive and taken together, form a longitudinal view in section of the retrievable well packer and seal assembly of the invention showing the seal assembly relaxed and the packer slips retracted as the packer is released and is ready for retrieval from a well bore;
FIG. 5 is a plan view of a barrel slip of the invention removed from the packer;
FIG. 6 is a plan interior view of a barrel slip of the invention removed from the packer;
FIG. 7 is a longitudinal view in section of the top wedge removed from the mandrel; and,
FIG. 8 is a longitudinal view in section of the bottom wedge removed from the mandrel.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the description which follows, like parts are marked throughout the specification and drawings with the same reference numerals, respectively. The drawings are not necessarily to scale and the proportions of certain parts have been exaggerated to better illustrate details and features of the invention. In the following description, the terms "upper," "upward," "lower," "below," "downhole" and the like, as used herein, shall mean in relation to the bottom, or furthest extent of, the surrounding wellbore even though the wellbore or portions of it may be deviated or horizontal. Where components of relatively well known design are employed, their structure and operation will not be described in detail.
Referring now to FIG. 1, a well packer 10 is shown in releasably set, sealed engagement against the bore 12 of a well casing 14. The tubular well casing 14 lines a well bore 16 which has been drilled through an oil and gas producing formation, intersecting multiple layers of overburden 18, 20 and 22, and then intersecting a hydrocarbon producing formation 2. The mandrel 34 of the packer 10 is connected to a tubing string 26 leading to a wellhead for conducting produced fluids from the hydrocarbon bearing formation 2 to the surface. The lower end of the casing which intersects the producing formation is perforated to allow well fluids such as oil and gas to flow from the hydrocarbon bearing formation 2 through the casing 14 into the well bore 12.
The packer 10 is releasably set and locked against the casing 14 by an anchor slip assembly 28. A seal element assembly 30 mounted on the mandrel 34 is expanded against the well casing 14 for providing a fluid tight seal between the mandrel and the well casing so that formation pressure is held in the well bore below the seal assembly and formation fluids are forced into the bore of the packer to flow to the surface through the production tubing string 26.
Referring now to FIGS. 2A-2C, which shows the packer as it is configured for running into the well for placement, the packer 10 is run into the well bore and set by hydraulic means. The anchor slip 100 of the anchor slip assembly 28 are first set against the well casing 14, followed by expansion of the seal element assembly 30. The packer 10 includes force transmitting apparati 104 and 58 with a cinch slip 102 which maintains the set condition after the hydraulic setting pressure is removed. The packer 10 is readily retrieved from the well bore by cutting the mandrel 34 and by a straight upward pull which is conducted through the mandrel and thereby permits the anchor slip 100 to retract and the seal elements 30A to relax, thus freeing the packer for retrieval to the surface. The entire packer and attached tubing is retrieved together.
The anchor slip assembly 28 and the seal element assembly 30 are mounted on a tubular body mandrel 34 having a cylindrical bore 36 defining a longitudinal production flow passage. The lower end of the mandrel 34 is firmly coupled to a bottom connector sub 38. The bottom connector sub 38 is continued below the packer within the well casing for connecting to a sand screen, polished nipple, tail screen and sump packer, for example. The central passage of the packer bore 36 as well as the polished bore, bottom sub bore, polished nipple, sand screen and the like are concentric with and form a continuation of the tubular bore of the upper tubing string 26.
In the preferred embodiment described herein, the packer 10 is set by a hydraulic actuator assembly 40, which comprises a piston 42 concentrically mounted on the mandrel 34, enclosing an annular chamber 44 which is open to the cylindrical bore 36 at port 46. The hydraulic actuator assembly 40 is coupled to the lower force transmitting assembly 104 for radially extending the anchor slip assembly 28 and seal element assembly 30 into set engagement against the well bore. Referring to FIG. 2B, the hydraulic actuator includes a tubular piston 42 which carries annular seals S for sealing engagement against the external surface of the mandrel 34. The piston 42 is also slidably sealed against the external surface of a bottom connector sub 38. The piston 42 is firmly attached to a lower wedge 88. Hydraulic pressure is applied through the inlet port 46 which pressurizes the annular chamber 44. As the chamber is pressurized, the piston 42 is driven upward, which thereby also moves the lower wedge upward.
Referring now to FIG. 8, the lower wedge 88 is positioned between the external surface of the mandrel 34 and the lower bore of the barrel slip 100 and features a number of upwardly facing frustoconical wedging surface cones 90. In the run in position, the lower wedge 88 and its cones 90 are fully retracted, and are blocked against further downward movement relative to the slip carder by the piston 42. The upper wedge 52 likewise has a number of downwardly facing frustoconical wedging surface cones 92.
The slip anchor assembly 28 includes a barrel slip 100 snugly fitted on the exterior surface of the upper and lower wedges 52 and 88. Referring now to FIGS. 5-8, the barrel slip 100 has a plurality of slip anchors 28A which are mounted for radial movement. A large number of slips, such as twelve or fourteen, is preferable. Each of the anchor slips includes lower gripping surfaces 106 and lower gripping surfaces 108 positioned to extend radially into the casing wall. Each of the gripping surfaces has horizontally oriented gripping edges (106A, 108A) which provide gripping contact in each direction of longitudinal movement of the packer 10. The gripping surfaces, including the horizontal gripping edges, are radially curved to conform with the cylindrical internal surface of the well casing bore against which the slip anchor members are engaged in the set position. As the packer is generally required to potentially withstand more loading in the upward direction, the barrel slip 100 has a longer lower face to resist upward movement. For purposes of this application, the "center" of the slip is the point along the axial length of the packer at which the gripping edges change directions, at 146.
The interior of the barrel slip 100 comprises a series of frustoconical surface cones 94, 98. The lower slip cones 94 are positioned adjacent to and generally complementary with the lower wedge cones 90, while the upper slip cones 98 are positioned adjacent to and generally complementary with the upper wedge cones 92. The number of lower slip cones 94 is higher than the number of upper slip cones 98, to complement the longer lower gripping surface 106 of the barrel slip. In this embodiment, the lower slip cones 94 are spaced equidistantly from each other. The upper slip cones 98 are also spaced equidistantly from each other.
Use of a barrel slip as shown here allows full circumferential contact with the casing. This design effectively spreads the slip-to-casing load over a large area and minimizes slip-to-casing contact stresses. With the use of a barrel slip, the casing is always urged into a circular cross section, even at full loads. Furthermore, the slip is designed to load uniformly such that equal loads are borne by all the slip teeth. This ensures minimum slip toth penetration into the casing wall.
The lower wedge cones 90 are not spaced identically to the corresponding lower slip cones 94. Instead, the two uppermost lower wedge cones 90A, 90B are spaced just slightly farther apart than their corresponding slip cones 94A, 94B. Thereafter, moving downward, each wedge cone is spaced progressively farther apart. While this embodiment is shown with four lower wedge cones, any number of cones would be acceptable. The upper wedge 52 is designed similarly to the lower wedge, in that the gap between the upper wedge cones 92 is slightly larger than the gap between the corresponding slip cones 98. This embodiment is shown with two cones, but the inventive concept would work with any number of cones, as long as the cones are spaced progressively further apart, with the smallest gap being between the lowest two upper wedge cones.
One of the inventive concepts disclosed in this application is the use of progressive loading of the slip. That is, the slip is loaded against the casing well near the longitudinal center of the slip first, then as load on the slip increases, the rest of the slip is progressively loaded against the casing wall from the longitudinal center out to the outer edge. The preferred embodiment described herein uses a constant gap between cones on the slip, and progressively broader gaps on the wedges. However, as is readily apparent, there are any number of combinations of gapping in the slip cones and wedge cones that can achieve the desired result. For example, the gaps between the wedge cones could be uniform, and the gaps between the slip cones could be progressively smaller from the center to the upper and lower edges. Any combination of slip cones and wedge cones that would result in the wedge cones being slightly progressively farther longitudinally removed from their corresponding slip cones, as viewed from the center to the upper and lower edges of the slip, would achieve the desired result. While this preferred embodiment is shown using a barrel slip, the other inventive concepts of this application could be used with other types of slips.
The slip carrier is releasably coupled to the lower wedge 88 by anti-preset shear screws. According to this arrangement, as the piston 42 is extended in response to pressurization through the port 46, the lower wedge 88, anchor slip assembly 28, and upper force transmitting assembly 58 are extended upwardly toward the seal element assembly 30. The upper force transmitting assembly comprises an element retainer collar 68 which is coupled to the upper wedge 52.
The seal element assembly 30 is mounted directly onto an external support surface 54 of the mandrel 34. The seal element assembly 30 includes an upper outside packing end element 30A, a center packing element 30B and a lower outside packing end element 30C. The upper end seal element 30A is releasably fixed against axial upward movement by engagement against an upper backup shoe 56, which in turn is connected to a cover sleeve 80. The upper backup shoe 56 and cover sleeve 80 are movably mounted on the mandrel 34 for longitudinal movement from a lower position, as shown in FIG. 2A, to an upper position (FIG. 3A) which permits the seal element assembly to travel upwardly along the external surface of the mandrel 34. In this arrangement, the seal element assembly undergoes longitudinal compression by the upper force transmitting assembly 58 until a predetermined mount of compression and expansion have been achieved.
Sealing engagement is provided by prop apparatus 60 which is mounted on the mandrel 34. In the preferred embodiment, the prop apparatus is a radially stepped shoulder member 61 which is integrally formed with the mandrel, with the prop surface 64 being radially offset with respect to the seal element support surface 54. In this arrangement, the prop apparatus 60 forms a part of the mandrel 34. The seal element prop surface 64 is preferably substantially cylindrical, and the seal element support surface 54 is also preferably substantially cylindrical. As can be seen in FIG. 2A, the seal element prop surface 64 is substantially concentric with the seal element support surface 54.
The ramp member 66 has an external surface 74 which slopes transversely with respect to the seal element support surface 54 and the seal element prop surface 64. Preferably, the slope angle as measured from the seal element support surface 54 to the external surface 74 of the ramp member 66 is in the range of from about 135 degrees to about 165 degrees. The purpose of the ramp surface is to provide a gradual transition to prevent damage to the upper seal element 30A as it is deflected onto the radially offset prop surface 64.
Referring to FIG. 2A, a transitional radius R1 is provided between the mandrel surface 54 and the sloping ramp surface 74, and a second radius R2 is provided between the ramp surface 74 and the radially offset prop surface 64. The two radius surfaces R1, R2 complement each other so that there is a smooth movement of the upper end element seal 30A from the mandrel surface 54 to the radially offset prop surface 64 without damage to the seal element material. For a slope angle A of 135 degrees, a relatively small radius of transition R1 of 0.06 inch radius is provided, and the second, relatively large radius is approximately 0.5 inch radius. According to this arrangement, a gently sloping ramp surface 74 provides an easy transition for the preloaded upper end seal element 30A to be deflected onto the radially offset prop surface 64. As the slope angle is increased, it becomes more important to radius the corners of the transition, and the specific radius values are determined based primarily on the size of the packer.
As shown in FIG. 2A, the upper outside seal element 30A has a substantially shorter longitudinal dimension than the central seal element 30B and the lower outside seal element 30C. The longitudinal dimension of the prop surface 64 is selected so that the upper outside seal element 30A is fully supported and the central seal element 30B is at least partially supported on the radially offset prop surface 64 in the set, expanded position, as shown in FIG. 3A. Even though the lower outside seal element 30C and the central seal element 30B may be subjected to longitudinal excursions as a result of pressure fluctuations, the sealing engagement of the upper outside seal element 30A is maintained at all times.
The lower and upper outside seal elements are reinforced with metal backup shoe 70 and 56, respectively. The metal backup shoes 70 and 56 provide a radial bridge between the mandrel 34 and the well casing 14 when the seal element assembly is expanded into engagement against the internal bore sidewall of the well casing, as shown in FIG. 3A. The purpose of the metal backup shoes is to bridge the gap between the mandrel and the casing and provide a support structure for the outside seal elements 30A and 30C, to prevent them from extruding into the annulus between the mandrel and the well casing.
The dimensions of the seal elements and the prop surface OD are selected to provide a minimum of 5 percent reduction in radially compressed thickness to a maximum of 30 percent reduction in radially compressed thickness as compared with the lower outside seal element 30C when compressed in the set position, for example as shown in FIG. 3A.
The backup shoes are preferably constructed in the form of annular metal discs, with the inside disc being made of brass and the outer metal disc being made of Type 1018 mild steel. Both metal discs are malleable and ductile, which is necessary for a tight conforming fit about the outer edge of the outside seal elements 30A and 30C.
The upper force transmitting apparatus 58 which applies the setting force to the seal element package includes a lower element retainer ring 72 mounted for longitudinal sliding movement along the seal element support surface 54 of the mandrel 34. An element retainer collar 68 is movably mounted on the external surface of the retainer ring 72 for longitudinal shifting movement from a retracted position (FIG. 2A) in which the seal elements are retracted, to an extended position (FIG. 3A) in which the seal elements are deployed.
The retainer ring 72 and element retainer collar 68 have mutually engageable shoulder portions 72A, 68A, respectively, for limiting extension of the element retainer collar along the external surface of the retainer ring. A split ring 76 is received within an annular slot 78 which intersects the external surface 54 of the mandrel 34. The split ring 76 limits retraction movement of the lower element retainer ring 72, thus indirectly limiting retraction movement of the element retainer collar 68, as shown in FIG. 4A.
Referring again to FIG. 2, the packer includes a locking assembly 148, which comprises the piston 42, mandrel 34, bottom connector sub 38, and cinch slip 102. The piston 42 concentrically and slidably fits over a portion of the bottom connector sub 38, as well as a portion of the mandrel 34. The piston is sealingly and concentrically fitted against the mandrel 34 as well as the bottom connector sub using seals S. The piston 42 further concentrically fits around a cinch slip 102, which in turn fits concentrically around the bottom connector sub 38. The outer surface 110 of the cinch slip is composed of a series of ridges, which are complementary to a series of ridges on the inner surface 112 of the piston, thereby interlocking the cinch slip and the piston. The piston 42 is further connected to the cinch slip 102 by pin 114.
The piston 42 and the bottom connector sub 38 define an annular gap 116, in which the cinch slip 102 is fitted. On the outer surface 118 of the bottom connector sub in the region from a radially offset shoulder 120 downward to a point proximate the lower end of the cinch slip 122 comprises a series of free radially spaced sharp tubular angular ridges. These ridges are complementary to ridges on the inner surface of the cinch slip. The complementary ridges on the bottom connector sub 38 and the cinch slip 102, together with the snug fit of the cinch slip 102 around the bottom connector sub 38, allow the cinch slip 102 to be forcibly moved upward with respect to the bottom connector sub 38, while not allowing the cinch slip 102 to move back downward with respect to the bottom connector sub 38. Upward travel of the cinch slip 102 with respect to the bottom connector sub 38 is limited by the radially offset shoulder 120. The cinch slip 102 is initially installed at the bottom of the annular gap 116, and sets on a wave spring 150.
A stop ring assembly 124 is positioned on the bottom connector sub 38 below the cinch slip 102, and connected to the cinch slip with a shear pin 126. The stop ring assembly 124 is set on a radially reduced offset surface 128 of the bottom connector sub, and is prevented from upward movement with respect to the bottom connector sub 38 by shoulder 130 which is complementary to shoulder 124A of the stop ring assembly.
Referring now to FIGS. 3A-3C, once the packer has been run in and positioned in the desired location, fluid is forced into the annular chamber 44 under pressure, thereby causing the piston 42 to be forced upward. The piston in turn forces the entire anchor slip assembly 28 and upper force transmitting assembly 58 to move upward, forcing the retainer ring 72 and element retainer collar 68 upward. This in turn forces the lower backup shoe 70 upward against the seal element assembly 30. The seal element assembly moves upward, moving elements 30A and 30B up the ramp member 66 and onto the prop surface 64, moving the upper backup shoe 56 and the cover sleeve 80 upward ahead of it. When the shoulder 82 of the cover sleeve 80 contacts the radially offset shoulder 62 on the mandrel 34 and can move no further upward, the seal assembly 30 is compressed between the backup shoes and the seals expand radially, sealing the annulus around the packer.
Once the seal assembly 30 is fully deployed, the upper wedge 52 and lower wedge 88 begin to move towards each other. See FIG. 3B. As described above, the wedge cones 90, 92 are generally complementary to the slip cones 94, 98, wherein the wedge cones are spaced progressively further distances apart, as viewed from the centermost to outermost cones. As the wedges 52, 88 are forced towards each other, the end cones of the wedges 90A, 92A which mate with the centermost cones of the slip 94A, 98A make contact first. As the wedges continue towards each other, the slip 100 is forced out into engaging contact with the well casing 14. As the centermost pair of cones are the only ones in actual contact, the center of the slip is loaded first. As greater forces are exerted on the wedges, the wedges will deform slightly and the next cones of the wedges 90B, 92B will make contact with their matching slip cones 94B, 98B. As can be seen, as the wedges are loaded higher and higher, more wedge cones come into bearing contact with the slip. The standoff between the cones of the wedges is controlled very precisely such that slight elastic yielding takes place by deforming the wedge inwardly.
This design effectively allows initial setting of the packer with very little slip tooth contact area of the upper and lower gripping surface 108, 106. This permits the slip 100 to quickly get a good grip into the casing wall. Subsequent higher loading brings more and more slip teeth 132 on the gripping surface to bear and prevents overstressing the casing. Loading is continued until all the edges 106A, 108A of the gripping surface 106, 108 are firmly engaged with the wall of the casing.
This design may also be used with a plurality of individual slips in place of the barrel slip. Further, the progressively gapped cones may be on the slip, with the uniformly gapped cones on the wedges. Further, both sets of cones may have varying gaps, as long as the centermost cones of the slips are engaged first, followed by the next nearest cones, and so on, as the wedges are progressively loaded.
Referring now to FIG. 3C, as the piston 42 is being moved upward in response to the pressurizing of the annular chamber 44, the piston 42 pulls cinch slip 102 upward along the bottom connector sub 38, shearing shear pin 126. As the cinch slip 102 moves upward, the fine ridges 134 on the inner surface 117 of the cinch slip 102 are forced over the fine ridges 136 on the surface 118 of the bottom connector sub 38. The cinch slip 102 is thereby pulled upward with respect to the bottom connector sub 38 until the upper end 123 of the cinch slip 102 contacts the radially offset shoulder 120. Once moved upward with respect to the bottom connector sub, the cinch slip is prevented from moving downward again by the opposing ridges 134, 136 of the cinch slip and the bottom connector sub. Hence, once pressure is released from the annular chamber 44, the packer 10 will stay fully deployed, as the cinch slip 102 will not allow the piston 42, anchor slip assembly 28, upper force transmitting assembly 58 and seal assembly 30 from moving back downward with respect to the mandrel 34 and bottom connector sub 38. The cinch slip thereby helps ensure that no premature release of the packer occurs and that it remains locked in its deployed position. Indeed, there is no way to move the cinch slip back downward with respect to the bottom connector sub without literally dismantling the packer.
This embodiment as described above has been deployed and tested, and shown to be able to withstand pressure differentials of 15,000 psi and temperatures to 600° F. without moving longitudinally in the well.
Referring now to FIGS. 4A-4C, to release the packer, a cutting tool (not shown) is lowered into the mandrel 34 and set down on internal shoulder 138. The full circumference of the mandrel 34 is then cut at a level proximate the port 46. At this point, if there is any load on bottom connector sub 38, the bottom connector sub will be pulled downward. Alternatively, the tubing string 26 and the mandrel 34 can be pulled upward. Now that the mandrel 34 is cut, the mandrel 34 and the bottom connector sub 38 can move axially away from each other. As they move apart, the piston 42, which is securely connected to the cinch slip 102, which in turn is securely held in position on the bottom connector sub 38, is pulled downward with respect to the mandrel 34. As the piston moves downward, the upper and lower wedges 52, 88 are moved axially apart from each other, allowing the slip 100 to release. As the piston 42 is moved further downward with respect to the mandrel 34, the upper force transmitting assembly 58 is pulled downward, and the sealing assembly 30 thereby relaxes and move back down off of the prop surface 64 and onto the support surface 54.
The downward movement of the piston 42 with respect to the mandrel 34 is limited by set screw 140 of the upper wedge 52, which contacts a stop shoulder 142. At this point, as the slips and seal assembly are fully retracted, and as the piston is still connected to both the mandrel and the bottom connector sub, the entire packer can be pulled upward and out of the well together.
As the mandrel 34 is pulled upward, the radially reduced support surface 54 of the mandrel 34 provides an annular pocket into which the seal elements are retracted upon release and retrieval of the packer. That is, upon release and upward movement of the mandrel 34, the seal elements 30A, 30B are pushed off of the prop surface 64 and slide onto the lower mandrel seal support surface 54. Thus the seal elements are permitted to expand longitudinally through the annular pocket, and away from the drift clearance thereby permitting unobstructed retrieval.
Thus, the invention is able to meet all the objectives described above. The foregoing description and drawings of the invention are explanatory and illustrative thereof, and various changes in sizes, shapes, materials, and arrangement of parts, as well as certain details of the illustrated construction, may be made within the scope of the appended claims without departing from the true spirit of the invention. Accordingly, while the present invention has been described herein in detail to its preferred embodiment, it is to be understood that this disclosure is only illustrative and exemplary of the present invention and is made merely for the purposes of providing and enabling disclosure of the invention. The foregoing disclosure is neither intended nor to be construed to limit the present invention or otherwise to exclude any such embodiments, adaptations, variations, modifications, and equivalent arrangements, the present invention being limited only by the claims appended hereto and the equivalents thereof. | In a retrievable packer adapted for service under high temperature and high pressure operating conditions, the packer is purpose-designed as a cut-to-release packer. That is, this retrievable packer has no built-in release mechanism. An internal cinch slip is used to retain the packer in its set position and thereby prevent the accidental release of the packer. The only way it can be released is by severing the mandrel. The cut point is opportunely designed so that the mandrel is severed in a precise location such that not only is the packer released, but all the packer and tail pipe are then retrievable as a unit. The primary advantage of a cut-to-release packer is that it can withstand extreme tubing loads occurring during production and stimulation. | 4 |
FIELD OF THE INVENTION
The present invention involves the use of dimethylsilicone fluids of moderate viscosity and/or di-alkyl or di-cycloalkyl or alkyl-cycloalkyl, or mixtures thereof, of di-end-capped polypropylene oxides or of ester compounds in combination with cyclic hydrocarbons to produce very high shear strength elastohydrodynamic (EHD) traction fluids and to modify the low temperature viscometric properties of the mixed fluids without adversely affecting the very high elastohydrodynamic shear strength or traction coefficients of the very high shear strength cyclic hydrocarbon fluid in the resulting mixed fluids with improved low temperature viscosity.
BACKGROUND OF THE INVENTION
Elastohydrodynamic traction drives are power transmission devices that operate by transmitting torque through a thin elastohydrodynamic film of fluid between nominally-smooth, rolling-sliding, highly-loaded contacts. The efficient transfer of torque relies upon the high-stress shear strength of the fluid used to lubricate the surfaces in these high-stress elastically-deformed contacts. Fluids with very high elastohydrodynamic shear strength, or high traction coefficients, enable the most efficient transfer of torque through these contacts from one surface to the other. Thus, the shear strength properties of the fluid under the EHD contact operational conditions effectively dictate the sizing of the device for a given power or torque transfer requirement. Or, in any given size of an EHD traction transmission, determines the loading of the contact, the contact stress, required to produce a required torque through the device and thus has a large impact on the durability of the traction drive components. Prior art fluids are described in U.S. Pat. No. 7,645,395 and references therein.
SUMMARY OF THE INVENTION
The present disclosure provides for, in one embodiment, a lubrication fluid including a dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination with a polycyclic hydrocarbon fluid. The dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
The present disclosure provides for, in another embodiment, a lubrication fluid including dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination with oil-soluble di-end-capped polypropyleneoxide compounds and a polycyclic hydrocarbon fluid. The dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
The present disclosure provides for, in yet another embodiment, the lubrication fluid including a dimethylsiloxane compound having a viscosity range of 20 cSt at 77° F. or greater in combination with a polycyclic hydrocarbon fluid and an ester compound independently selected from: a branched alkyl ester, a cycloester, a cycloalkyl ester and combinations thereof. The dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups.
DETAILED DESCRIPTION OF THE EMBODIMENTS
The present invention provides for formulations for lubricants of high elastohydrodynamic shear strength or traction coefficients and good low temperature rheology. This combination of properties is generally known in the art to be very difficult to achieve. Historically, achieving fluid formulations with good low temperature rheological properties has always compromised elastohydrodynamic shear strength to some degree. The various formulation embodiments described herein eliminate these losses and in some cases the formulation scheme actually is found to improve elastohydrodynamic shear strength under certain operational conditions in elastohydrodynamic traction contacts while achieving good low temperature rheological properties suitable for all-weather operations.
In one embodiment, the lubrication fluid comprises a dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination with a polycyclic hydrocarbon fluid wherein the dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
In another embodiment, the lubrication fluid consists essentially of dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination with a polycyclic hydrocarbon fluid, wherein the dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
In yet another embodiment, the lubrication fluid comprises dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination with oil-soluble di-end-capped polypropyleneoxide compounds and a polycyclic hydrocarbon fluid, wherein the dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
In still yet another embodiment, the lubrication fluid consists essentially of dimethylsiloxane fluid having a viscosity of 20 cS at 77° F. or greater in combination in combination with oil-soluble di-end-capped polypropyleneoxide compounds and a polycyclic hydrocarbon fluid, wherein the dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups so to modify the low temperature properties of polycyclic hydrocarbons fluids. In one embodiment, the dimethylsiloxane fluid has a viscosity of 20 cS but not greater than 50 cS at 77° F.
In yet another embodiment, the lubrication fluid comprises a dimethylsiloxane compound having a viscosity range of 20 cSt at 77° F. or greater in combination with a polycyclic hydrocarbon fluid and an ester compound independently selected from: a branched alkyl ester, a cycloester, a cycloalkyl ester and combinations thereof. The dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups.
In still yet another embodiment, the lubrication fluid consists essentially of a dimethylsiloxane compound having a viscosity range of 20 cSt at 77° F. or greater in combination with a polycyclic hydrocarbon fluid and an ester compound independently selected from: a branched alkyl ester, a cycloester, a cycloalkyl ester and combinations thereof. The dimethylsiloxane fluid does not contain more than 10 wt. % of functional groups other than methyl functional groups.
For the purposes of this disclosure, consists essentially of excludes the inclusion of any component that materially changes the low temperature properties of polycyclic hydrocarbons fluids.
It was unexpectedly found that addition of dimethylsiloxane fluids to polycyclic hydrocarbons fluid with or without oil-soluble di-end-capped polypropylene oxide compounds results in a lubrication fluid having improved low temperature properties without degrading the desired elastohydrodynamic shear strength properties or traction coefficients of the binary or ternary lubrication fluid relative to the polycyclic hydrocarbons fluid alone.
It was further was unexpectedly found that addition of dimethylsiloxane fluids to polycyclic hydrocarbons fluid with branched ester, cycloester or cycloalkyl ester compounds results in a lubrication fluid having improved low temperature properties without degrading the desired elastohydrodynamic shear strength properties or traction coefficients of the binary or ternary lubrication fluid relative to the polycyclic hydrocarbons fluid alone.
Base Oils
The present invention provides for a lubrication fluid based on a polycyclic hydrocarbon fluid which exhibits good shear strength but poor low temperature properties. In some embodiments, the polycyclic hydrocarbon fluid is a perhydro dimer of alpha-methylstyrene. In some another embodiments, the polycyclic hydrocarbon fluid is a perhydro linear dimer of alpha-methylstyrene.
In one embodiment, the polycyclic hydrocarbon fluid may be combined with a dimethylsiloxane fluid having a viscosity of at least 20 cS at 77° F. or greater wherein the dimethylsiloxane fluid contains no more than 10 wt. % of functional groups other than methyl functional groups. The dimethylsiloxane fluid may be used at an amount ranging from 0.1 wt. to 25 wt. %.
In another embodiment, the polycyclic hydrocarbon fluid may be combined with a dimethylsiloxane fluid having a viscosity of at least 20 cS at 77° F. or greater and oil-soluble di-end-capped polypropylene oxide compounds wherein the dimethylsiloxane fluid contains no more than 10 wt. % of functional groups other than methyl functional groups. The dimethylsiloxane fluid may be used at an amount ranging from 0.1 wt. to 25 wt. %. The oil-soluble di-end-capped polypropylene oxide compound may be used at an amount ranging from 0.1 wt. to 25 wt. %. In one such embodiment, the di-end-capped polypropylene oxide compounds may contain alkyl groups, cycloaliphatic rings, aromatic rings or combinations of these organic groups as the end-capping organic groups. In one embodiment, the end-capping organic groups have one to ten carbon atoms.
In another embodiment, the polycyclic hydrocarbon fluid may be combined with a dimethylsiloxane fluid having a viscosity of at least 20 cS at 77° F. or greater and branched ester, cycloester or cycloalkyl ester compounds wherein the dimethylsiloxane fluid contains no more than 10 wt. % of functional groups other than methyl functional groups. The dimethylsiloxane fluid may be used at an amount ranging from 0.1 wt. to 25 wt. %. The branched ester, cycloester, cycloalkyl ester compounds and combinations thereof may be used at an amount ranging from 0.1 wt. to 25 wt. %.
In one embodiment, the ester compound is a branched alkyl ester having 6 to 12 carbon atoms in the branched alkyl group and 3 to 4 ester groups. In one embodiment, the branched alkyl ester has at least two methyl groups distributed along the backbone of the branched alkyl ester. In another embodiment, the branched alkyl ester has at least one branching methyl or branching alkyl group per two carbon atoms located along the backbone of the branched alkyl ester. In one embodiment, the branched alkyl ester is trimethylhexane trimethoxypropane ester. In another embodiment, the branched alkyl ester is trimethylhexane pentaerithritol ester.
In one embodiment, the ester compound is a cycloester or cycloalkyl ester compound selected from cyclohexyl group or alkyl cyclohexyl group having 6 to 10 carbon atoms and 3 to 4 ester groups. In one embodiment, the cycloester compound independently includes tri-(cyclohexyl)trimethoxypropane and tri-(cyclohexyl)pentaerithritol. In another embodiment, the cycloalkyl ester compound independently includes (alkyl branched-cyclohexyl)trimethoxypropane and tri-(alkyl branched-cyclohexyl)pentaerithritol. Examples include (methyl branched-cyclohexyl)trimethoxypropane and tri-(methylcyclohexyl)pentaerithritol. In some such embodiments, the number of methyl groups attached to the cyclohexyl group ranges from 1 to 3.
In one embodiment, the dimethylsiloxane fluid may have other functional groups including, but are not limited to, higher alkyl groups, cycloaliphatic rings, aromatic rings or a combination of these non-methyl organic groups. In yet another embodiment, the dimethylsiloxane fluids may be produced as purely dimethyl-derivatives.
The viscosity grades of such dimethylsiloxane fluids have the added advantage of being relatively non-volatile at typical lubricant or transmission operation temperatures in a EHD traction drive or traction drive transmission of at least 20 cS at 77° F. and higher. For example, typically 10 cSt (at 77° F.) dimethylsiloxane has a volatility of 50 wt % at 150° C. relative to 20 cSt dimethylsiloxane which typically has only a 5% volatility at 150° C.
In one embodiment, the dimethylsiloxane fluid has a viscosity greater than 20 cSt at 77° F. but not greater than 50 cS at 77° F. and may be used at an amount ranging from 0.1 wt. to 25 wt. %. In one embodiment, the dimethylsiloxane fluid has a viscosity greater than 25 cSt at 77° F. but not greater than 50 cS at 77° F. and may be used at an amount ranging from 0.1 wt. to 25 wt. %. In one embodiment, the dimethylsiloxane fluid has a viscosity greater than 30 cSt at 77° F. but not greater than 50 cS at 77° F. and may be used at an amount ranging from 0.1 wt. to 25 wt. %. In yet another embodiment, the dimethylsiloxane fluid has a viscosity of greater than 40 cSt at 77° F. but not greater than 50 cS at 77° F. and may be used at an amount ranging from 0.1 wt. to 25 wt. %. The higher viscosity versions are contemplated to be appropriate when higher viscosity grade elastohydrodynamic traction fluid lubricants are desired whereby higher formulation concentrations are needed to significantly modify the low temperature rheology of the finished fluids which results in finished fluids with kinematic viscosities of about 4.0 cSt or above, measured at 100° C.
The lubrication fluids described herein can serve as base fluids for the formulation of high elastohydrodynamic shear strength fluids for use in elastohydrodynamic continuously or infinitely variable transmission or in elastohydrodynamic traction drives in general. To these combination base fluids appropriate lubricant performance additives may be added to complete the formulation of the transmission or traction drive fluid. These additives may include antioxidants, antiwear agents, anti-corrosion agents, anti-foamants, anti-rust agents, detergents, dispersants, extreme-pressure agents, friction modifiers, seal swell agents and/or viscosity modifier additives.
The various embodiments of the lubrication fluids described herein allow for production of useful fully-formulated EHD traction fluids having kinematic viscosities of from about 3.7 to 4.5 cS at 100° C. and low temperature dynamic viscosities ranging from 28,000 cP down to about 5,000 cP which do not compromise EHD shear strength properties to any appreciable degree.
The following examples describe various embodiments of the invention. Other embodiments within the scope of the claims herein will be apparent to one skilled in the art from consideration of the specification or practice of the invention as disclosed herein. It is intended that the specification, together with the examples, be considered exemplary only, with the scope and spirit of the invention being indicated by the claims which follow the examples. In the examples, all percentages are given on a weight basis unless otherwise indicated.
In the below examples, the following abbreviations are used: Sep=Separation; No Sep=Separation; SCL—Slightly Cloudy; and Cl—Cloudy
Comparative Example
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer
Component
wt. %
Perhydro-alpha-Methylstyrene Dimer
96.8
Poly-Propylene Oxide Fluid
Dimethylsiloxane, 20 cSt @ 77 F.
Dimethylsiloxane, 30 cSt @ 77 F.
Performance Additive Package
3.0
Anti-Foamant Package
0.2
100.00
Test
Units
CS 40 C., cS
20.15
CS 100 C., cS
3.66
VI
31
Anton Paar SVM, −20 C., cP
4813
Anton Paar SVM, −30 C., cP
31182
Appearance (24 hrs @ temperature)
70 F.
C
35 F.
C
0 F.
No Sep
Example 1
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer and Poly-Propylene Oxide
Component
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
91.80
86.80
81.80
Poly-Propylene Oxide Fluid
5.00
10.00
15.00
Dimethylsiloxane, 20 cSt @ 77 F.
Performance Additive Package
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
100.00
100.00
100.00
Test
Unit
Unit
Unit
CS 40 C., cS
18.63
20.09
19.69
CS 100 C., cS
3.66
3.89
3.96
VI
63
74
92
Anton Paar SVM, −20 C., cP
4440
3258
3333
Anton Paar SVM, −30 C., cP
27609
20094
23088
Brookfield, −30 C., cP
Appearance, 24 hrs @ temp
70-75 F.
C
C
C
35-40 F.
C
C
C
0-5 F.
No Sep
No Sep
No Sep
Example 2
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer, Poly-Propylene Oxide and Dimethylsiloxane, 20 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
86.80
81.80
76.80
71.80
66.80
81.80
76.80
Poly-Propylene Oxide Fluid
5.00
5.00
5.00
5.00
5.00
10.00
10.00
Dimethylsiloxane, 20 cSt @ 77 F.
5.00
10.00
15.00
20.00
25.00
5.00
10.00
Performance Additive Package
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
18.80
18.65
17.32
16.46
14.69
19.50
18.55
CS 100 C., cS
3.77
3.92
4.04
4.10
3.98
4.05
4.08
VI
79
103
136
150
183
105
121
Anton Paar SVM, −20 C., cP
2547
1672
1166
774
641
2149
1541
Anton Paar SVM, −30 C., cP
13818
8689
6026
3759
3153
11471
7886
Brookfield, −30 C., cP
9118
7728
Appearance, 24 hrs @ temp
70-75 F.
C
C
C
C
C
C
C
35-40 F.
C
C
C
C
C
C
C
0-5 F.
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
71.80
66.80
61.80
76.80
71.80
66.80
61.80
56.80
Poly-Propylene Oxide Fluid
10.00
10.00
10.00
15.00
15.00
15.00
15.00
15.00
Dimethylsiloxane, 20 cSt @ 77 F.
15.00
20.00
25.00
5.00
10.00
15.00
20.00
25.00
Performance Additive Package
3.00
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
17.59
16.48
14.92
18.47
17.22
17.20
17.14
16.77
CS 100 C., cS
4.15
4.15
4.13
4.00
4.03
4.22
4.37
4.49
VI
143
163
197
114
137
158
177
198
Anton Paar SVM, −20 C., cP
914
706
624
2165
1398
953
811
689
Anton Paar SVM, −30 C., cP
4384
3272
2859
12378
7440
4667
3646
2804
Brookfield, −30 C., cP
Appearance, 24 hrs @ temp
70-75 F.
C
C
C
C
C
C
C
C
35-40 F.
C
C
C
C
C
C
C
C
0-5 F.
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
Example 3
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer, Poly-Propylene Oxide and Dimethylsiloxane, 30 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
86.80
81.80
76.80
71.80
66.80
81.80
76.80
Methylstyrene Dimer
Poly-Propylene Oxide Fluid
5.00
5.00
5.00
5.00
5.00
10.00
10.00
Shin Etsu DC200, 30 cSt
5.00
10.00
15.00
20.00
25.00
5.00
10.00
Performance Additive
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Package
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
19.42
18.36
18.05
17.26
17.35
18.94
19.56
CS 100 C., cS
3.81
4.03
4.20
4.32
4.54
4.00
4.32
VI
73
118
141
168
192
107
131
Anton Paar SVM, −20 C., cP
3225
2078
1778
2270
1818
Anton Paar SVM, −30 C., cP
19186
11296
9398
12944
9756
Appearance, 24 hrs @ temp
70-75 F.
C
C
C
C
C
C
C
35-40 F.
C
SCL
SCL
Sep
Sep
C
SCL
0-5 F.
No Sep
No Sep
No Sep
No Sep
No Sep
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
71.80
66.80
61.80
76.80
71.80
66.80
61.80
56.80
Methylstyrene Dimer
Poly-Propylene Oxide Fluid
10.00
10.00
10.00
15.00
15.00
15.00
15.00
15.00
Shin Etsu DC200, 30 cSt
15.00
20.00
25.00
5.00
10.00
15.00
20.00
25.00
Performance Additive
3.00
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Package
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
19.22
20.44
20.16
19.74
19.57
19.03
CS 100 C., cS
4.50
4.38
4.52
4.67
4.82
5.00
VI
155
126
143
163
181
209
Anton Paar SVM, −20 C., cP
2338
Anton Paar SVM, −30 C., cP
14450
Appearance, 24 hrs @ temp
70-75 F.
C
C
C
C
C
C
C
C
35-40 F.
Sep
Sep
Sep
C
CL
CL
CL
Sep
0-5 F.
No Sep
Example 4
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer, Poly-Propylene Oxide and Dimethylsiloxane, 50 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
86.80
81.80
76.80
71.80
66.80
81.80
76.80
Poly-Propylene Oxide Fluid
5.00
5.00
5.00
5.00
5.00
10.00
10.00
Dimethylsiloxane, 50 cSt @ 77 F.
5.00
10.00
15.00
20.00
25.00
5.00
10.00
Performance Additive Package
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
CS 40 C., cS
CS 100 C., cS
VI
Anton Paar SVM, −20 C., cP
Anton Paar SVM, −30 C., cP
Appearance, 24 hrs @ temp
70-75 F.
SCl
Sep
Sep
Sep
Sep
SCl
Sep
35-40 F.
Sep
Sep
Sep
Sep
Sep
Sep
Sep
0-5 F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
71.80
66.80
61.80
76.80
71.80
66.80
61.80
56.80
Poly-Propylene Oxide Fluid
10.00
10.00
10.00
15.00
15.00
15.00
15.00
15.00
Dimethylsiloxane, 50 cSt @ 77 F.
15.00
20.00
25.00
5.00
10.00
15.00
20.00
25.00
Performance Additive Package
3.00
3.00
3.00
3.00
3.00
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
CS 40 C., cS
21.000
CS 100 C., cS
4.42
VI
122
Anton Paar SVM, −20 C., cP
2713
Anton Paar SVM, −30 C., cP
17492
Appearance, 24 hrs @ temp
70-75 F.
Sep
Sep
Sep
C
Sep
Sep
Sep
Sep
35-40 F.
Sep
Sep
Sep
C
Sep
Sep
Sep
Sep
0-5 F.
No Sep
Example 5
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer with or without Poly-Propylene Oxide and with or without Dimethylsiloxane, 20 cSt @ 77° F. or 30 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
91.8
86.8
81.8
76.8
71.8
91.8
86.8
81.8
Methylstyrene Dimer
Poly-Propylene Oxide Fluid
5.0
10.0
15.0
20.0
25.0
Dimethylsiloxane, 20 cSt
5.0
10.0
15.0
@ 77 F.
Dimethylsiloxane, 30 cSt
@ 77 F.
Performance
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
Additive Package
Anti-Foamant Package
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
20.36
20.78
21.12
21.43
21.96
18.92
17.67
16.94
CS 100 C., cS
3.76
3.92
4.00
4.15
4.41
3.72
3.76
3.88
VI
46
66
73
90
110
68
100
124
Anton Paar SVM, −20 C., cP
4248
3798
3788
3857
3916
2907
1967
1447
Anton Paar SVM, −30 C., cP
26364
25216
25883
26634
27137
16999
11244
8057
Appearance (24 hrs
@ temperature)
70 F.
C
C
C
C
C
C
C
C
35 F.
C
C
C
C
C
C
C
C
0 F.
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
76.8
71.8
96.8
91.8
86.8
81.8
76.8
71.8
Methylstyrene Dimer
Poly-Propylene Oxide Fluid
20.0
25.0
Dimethylsiloxane, 20 cSt
5.0
10.0
15.0
20.0
25.0
@ 77 F.
Dimethylsiloxane, 30 cSt
@ 77 F.
Performance
3.0
3.0
3.0
3.0
3.0
3.0
3.0
3.0
Additive Package
Anti-Foamant Package
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
100.00
100.00
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
16.08
15.58
20.32
19.31
18.59
17.93
17.48
15.72
CS 100 C., cS
3.90
4.03
3.67
3.80
3.94
4.07
4.22
4.08
VI
141
167
31
74
106
129
153
171
Anton Paar SVM, −20 C., cP
1186
938
5161
3149
2388
1985
1534
956
Anton Paar SVM, −30 C., cP
6473
5207
33580
19169
13640
11172
7600
5352
Appearance (24 hrs
@ temperature)
70 F.
C
C
C
C
C
C
C
C
35 F.
C
C
C
C
C
C
C
C
0 F.
No Sep
No Sep
No Sep
No Sep
No Sep
No Sep
Sep
Sep
Example 6
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer and Dimethylsiloxane, 50 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-Methylstyrene Dimer
96.8
91.8
86.8
81.8
76.8
71.8
Poly-Propylene Oxide Fluid
Dimethylsiloxane, 50 cSt @ 77 F.
5.00
10.00
15.00
20.00
25.00
Performance Additive Package
3.00
3.00
3.00
3.00
3.00
3.00
Anti-Foamant Package
0.20
0.20
0.20
0.20
0.20
0.20
100.00
100.00
100.00
100.00
100.00
100.00
Test
Unit
Unit
Unit
Unit
Unit
Unit
CS 40 C., cS
20.32
19.80
20.20
19.80
19.50
CS 100 C., cS
3.67
3.87
4.23
4.08
4.34
VI
31
76
114
105
134
Anton Paar SVM, −20 C., cP
5161
3370
2785
Anton Paar SVM, −30 C., cP
33580
22050
16010
Appearance (24 hrs @ temperature)
70 F.
C
C
C
Sep
35 F.
C
CL
CL
0 F.
No Sep
No Sep
No Sep
Sep
Sep
Sep
Example 7
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer, Tri-Iso-C 9 Trimethoxylpropane Ester with or without Dimethylsiloxane, 20 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-
91.8
86.8
81.8
76.8
86.8
81.8
alpha-
Methylstyrene
Dimer
Tri-i-C9 TMP
5
5
5
5
10
10
ester
Dimethacone,
5
10
15
5
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
CS 40 C., cS
20.27
19.22
18.16
17.29
20.96
19.50
CS 100 C., cS
3.680
3.788
3.857
3.940
3.800
3.856
VI
33.2
73.9
103.5
125.2
42.2
79.5
Anton Paar
3696.2
2678.3
1711.6
1209.4
4352.4
2540.1
SVM, −20 C., cP
Anton Paar
22538
14748
8956
6366
26690
13574
SVM, −30 C., cP
Appearance
70-75 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
35-40 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
0-5 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-
76.8
71.8
81.8
76.8
71.8
66.8
alpha-
Methylstyrene
Dimer
Tri-i-C9 TMP
10
10
15
15
15
15
ester
Dimethacone,
10
15
5
10
15
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
CS 40 C., cS
18.62
17.73
21.49
20.17
19.06
18.26
CS 100 C., cS
3.934
4.023
3.886
3.956
4.017
4.123
VI
105.4
127.2
47.5
82.8
107.9
129.8
Anton Paar
1701.7
1115.8
4223
2578.3
1652.2
1094.1
SVM, −20 C., cP
Anton Paar
8369
5487
25637
13683
7833
4770
SVM, −30 C., cP
Appearance
70-75 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
35-40 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
0-5 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
91.8
86.8
81.8
76.8
86.8
81.8
Methylstyrene
Dimer
Tri-i-C9 TMP ester
5
5
5
5
10
10
Dimethacone, 30 cSt
5
10
15
5
@ 77 F.
Performance
3
3
3
3
3
3
Additive Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
CS 40 C., cS
20.27
19.74
19.14
18.72
20.96
20.16
CS 100 C., cS
3.680
3.875
4.029
4.171
3.800
3.956
VI
33.2
78.1
108.0
128.1
42.2
83.2
Anton Paar SVM, −20 C.,
3696.2
—
—
—
4352.4
—
cP
Anton Paar SVM, −30 C.,
22538
—
—
—
26690
—
cP
Appearance
70-75 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
35-40 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
0-5 F.
Clear, NS
Cldy, NS
Cldy, NS
Cldy, NS
Clear, NS
Cldy, NS
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
76.8
71.8
81.8
76.8
71.8
66.8
Methylstyrene
Dimer
Tri-i-C9 TMP ester
10
10
15
15
15
15
Dimethacone, 30 cSt
10
15
5
10
15
@ 77 F.
Performance
3
3
3
3
3
3
Additive Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
CS 40 C., cS
19.6
19.19
21.49
20.66
20.21
19.81
CS 100 C., cS
4.123
4.311
3.886
4.069
4.238
4.454
VI
111.3
135.4
47.5
91.1
114.9
140.9
Anton Paar SVM, −20 C.,
—
—
4223
2656
—
—
cP
Anton Paar SVM, −30 C.,
—
—
25637
14165
—
—
cP
Appearance
70-75 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
35-40 F.
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
Clear, NS
0-5 F.
Cldy, NS
Cldy, NS
Clear, NS
Clear, NS
Cldy, NS
Cldy, NS
Example 8
Lubrication Fluid Containing Perhydro-Alpha-Methylstyrene Dimer, Tri-Iso-C 9 Tpentaerithritol Ester with or without Dimethylsiloxane, 20 cSt @ 77° F.
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
91.8
86.8
81.8
76.8
71.8
66.8
86.8
81.8
76.8
Methylstyrene
Dimer
Tetra-i-C9 PE
5
5
5
5
5
5
10
10
10
ester
Dimethacone,
5
10
15
20
25
5
10
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
12.65
19.31
21.53
20.15
CS 100 C., cS
3.95
3.85
3.92
3.98
VI
56
81.7
51.7
86.6
Anton Paar
4601
2702.8
3734.9
2280.1
SVM, −20 C., cP
Anton Paar
27745
14793
21392
11614
SVM, −30 C., cP
Appearance
70-75 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
35-40 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
0-5 F.
clear NS
clear NS
cldy NS
cldy SEP
cldy SEP
cldy SEP
clear NS
clear NS
cldy NS
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
71.8
66.8
61.8
81.8
76.8
71.8
66.8
61.8
56.8
Methylstyrene
Dimer
Tetra-i-C9 PE
10
10
10
15
15
15
15
15
15
ester
Dimethacone,
15
20
25
5
10
15
20
25
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
22.07
20.68
CS 100 C., cS
4.04
4.1
VI
62.3
95.2
Anton Paar
3191.2
2048
SVM, −20 C., cP
Anton Paar
17219
9830
SVM, −30 C., cP
Appearance
70-75 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
35-40 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
0-5 F.
cldy SEP
cldy SEP
cldy SEP
clear NS
clear NS
cldy NS
cldy SEP
cldy SEP
cldy SEP
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
91.8
86.8
81.8
76.8
71.8
66.8
86.8
81.8
76.8
Methylstyrene
Dimer
Tetra-i-C9 PE
5
5
5
5
5
5
10
10
10
ester
Dimethacone,
5
10
15
20
25
5
10
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
20.63
21.57
CS 100 C., cS
3.78
3.92
VI
44.1
51.7
Anton Paar
4324
2902
SVM, −20 C., cP
Anton Paar
25671
16225
SVM, −30 C., cP
Appearance
70-75 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
35-40 F.
clear NS
cldy NS
cldy NS
cldy NS
cldy SEP
cldy SEP
clear NS
clear NS
cldy NS
0-5 F.
clear NS
cldy NS
cldy NS
cldy NS
cldy SEP
cldy SEP
clear NS
cldy NS
cldy NS
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
71.8
66.8
61.8
81.8
76.8
71.8
66.8
61.8
56.8
Methylstyrene
Dimer
Tetra-i-C9 PE
10
10
10
15
15
15
15
15
15
ester
Dimethacone,
15
20
25
5
10
15
20
25
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
21.48
CS 100 C., cS
3.98
VI
63.1
Anton Paar
3122
SVM, −20 C., cP
Anton Paar
16896
SVM, −30 C., cP
Appearance
70-75 F.
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
clear NS
35-40 F.
cldy NS
cldy SEP
cldy SEP
cldy NS
cldy NS
cldy NS
cldy SEP
cldy SEP
cldy SEP
0-5 F.
cldy SEP
cldy SEP
cldy SEP
clear NS
cldy NS
cldy SEP
cldy SEP
cldy SEP
cldy SEP
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
91.8
86.8
81.8
76.8
71.8
66.8
86.8
81.8
76.8
Methylstyrene
Dimer
Tetra-i-C9 PE
5
5
5
5
5
5
10
10
10
ester
Dimethacone,
5
10
15
20
25
5
10
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
20.5
20.93
CS 100 C., cS
3.74
3.85
VI
40.8
52.2
Anton Paar
4027
3540
SVM, −20 C., cP
Anton Paar
24316
20279
SVM, −30 C., cP
Appearance
70-75 F.
clear NS
clear NS
clear NS
clear NS
clear NS
cldy NS
clear NS
cldy NS
cldy SEP
35-40 F.
clear NS
cldy SEP
cldy SEP
cldy SEP
cldy SEP
cldy SEP
clear NS
cldy NS
cldy SEP
0-5 F.
clear NS
cldy SEP
cldy SEP
cldy SEP
cldy SEP
cldy SEP
clear NS
cldy SEP
cldy SEP
Component
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Wt. %
Perhydro-alpha-
71.8
66.8
61.8
81.8
76.8
71.8
66.8
61.8
56.8
Methylstyrene
Dimer
Tetra-i-C9 PE
10
10
10
15
15
15
15
15
15
ester
Dimethacone,
15
20
25
5
10
15
20
25
20 cSt @ 77 F.
Performance
3
3
3
3
3
3
3
3
3
Additive
Package
Anti-Foamant
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.2
Package
100
100
100
100
100
100
100
100
100
CS 40 C., cS
21.46
CS 100 C., cS
3.98
VI
63.1
Anton Paar
3150
SVM, −20 C., cP
Anton Paar
17197
SVM, −30 C., cP
Appearance
70-75 F.
cldy SEP
cldy SEP
cldy NS
clear NS
cldy NS
cldy SEP
cldy SEP
cldy SEP
cldy NS
35-40 F.
cldy SEP
cldy SEP
cldy SEP
clear NS
cldy SEP
cldy SEP
cldy SEP
cldy SEP
cldy SEP
0-5 F.
cldy SEP
cldy SEP
cldy SEP
clear NS
cldy SEP
cldy SEP
cldy SEP
cldy SEP
cldy SEP
It will be appreciated by those skilled in the art that changes could be made to the exemplary embodiments shown and described above without departing from the broad inventive concept thereof. It is understood, therefore, that this invention is not limited to the exemplary embodiments shown and described, but it is intended to cover modifications within the spirit and scope of the present invention as defined by the claims. For example, specific features of the exemplary embodiments may or may not be part of the claimed invention and features of the disclosed embodiments may be combined. Accordingly, reference should be made to the appended claims, rather than the foregoing specification, as indicating the scope of the disclosure. Unless specifically set forth herein, the terms “a”, “an” and “the” are not limited to one element but instead should be read as meaning “at least one”. | A lubrication fluid including cyclic hydrocarbons in combination with dimethylsilicone fluids and/or di-alkyl or di-cycloalkyl or alkyl-cycloalkyl, or mixtures thereof, and di-end-capped polypropylene oxides or highly branched esters to produce very high traction elastohydrodynamic (EHD) traction fluids and to modify the low temperature viscometric properties of the mixed fluids without adversely affecting the very high elastohydrodynamic shear strength or traction coefficients of the very high shear strength cyclic hydrocarbon fluid in the resulting mixed fluids with improved low temperature viscosity. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation under 35 USC §120 of PCT/EP2007/056415, filed 27 Jun. 2007, which is in turn entitled to benefit of a right of priority under 35 USC §119 from European patent application 06 11 6246.7, filed 28 Jun. 2006, the content of each of which is incorporated by reference as if fully recited herein.
TECHNICAL FIELD
The invention relates to a calibration weight arrangement for an electronic balance and in particular to a drive mechanism for a calibration weight arrangement.
BACKGROUND OF THE ART
Electronic balances are in many cases calibrated by means of an internal calibration weight. To perform a calibration, a calibration weight of a defined mass is brought into force-transmitting contact with the force-transmitting mechanism that is arranged in the force-measuring cell of a balance, whereupon a reference weight is determined. Based on this reference value, it is possible to adjust further weighing parameters of the balance. After the calibration has been successfully completed, the contact between the calibration weight and the force-transmitting mechanism is released again and the calibration weight is locked in a rest position. In this process, the calibration weight is moved from a rest position into a calibrating position and back by a transfer mechanism which includes at least one lifting element cooperating with a drive mechanism. In the calibrating position, the calibration weight is in force-transmitting contact with the force-transmitting device, while there is no force-transmitting contact in the rest position.
The known state of the art offers various types of lifting elements and versions of calibration weight arrangements.
A calibration weight which is disclosed in EP 0 468 159 B1 is moved vertically by pairs of wedge blocks sliding horizontally against each other and is thereby brought into force-transmitting contact with the force-transmitting device of the balance. This lifting element is driven by way of a motor and a horizontally oriented spindle which is connected to the wedge blocks.
A device described in EP 0 955 530 A1 likewise effects a vertical lifting and lowering of a calibration weight. The weight rests on a seat which is moved by an electrically driven lifting element.
An arrangement is described in DE 203 18 788 U1, where a monolithically formed calibration weight is lifted and lowered by a ramp-like lifting element, wherein the lifting element is actuated by a linear drive and performs a kind of slanted translatory movement.
In many balances, the calibration weight arrangement and the force-transmitting device are arranged behind one another, as is disclosed in EP 0 955 530 A1. However, the calibration weight can also be split up for example into two calibration weights and can be attached laterally to the force-transmitting device, like the cylindrical calibration weights disclosed in EP 0 789 232 B1. The two identical weights are arranged on two opposite sides of the force-transmitting device. Two different mechanisms for moving the calibration weights are described. In the first case, the calibration weight which is equipped with a guide pin is resting on a calibration weight seat configured as a support. To perform a calibration, the calibration weight seat which is hinged on one side is tilted, whereby the calibration weight is lowered and set onto two calibration weight carriers that are connected to the force-transmitting device and are configured as rods or levers. In a second version, the weight in its rest position is held on a calibration weight seat that is arranged between the calibration weight carriers that are connected to the force-transmitting device. To perform a calibration, the calibration weight is brought into contact with the calibration weight carriers through a vertical downward movement of the calibration weight seat.
A calibration weight arrangement is disclosed in DE 201 19 525 U1 with a lifting device for a calibration mechanism which includes two angled levers with fulcrum mounts fixed in the housing, whose vertical lever arms are coupled to each other by a horizontal slide and on whose horizontal lever arms the calibration weight is seated.
The aforementioned lifting elements are generally driven by servo motors. The disadvantage in using a servo motor is that it uses a comparatively large amount of space in the force-measuring cell of the balance, whereby the force-measuring cell as well as the balance itself is unnecessarily enlarged.
Especially in highly sensitive electronic balances, the weighing result is influenced and even changed by electrostatic charges and interactions. The servo motors which are used to drive the transfer mechanisms contain electrically non-conductive gearbox components which generate electrostatic charges through friction which occurs during operation. The resulting electrostatic fields, but also electromagnetic fields of conventional electric motors, are strong enough to influence the weighing result, in particular in balances of high sensitivity.
Almost always, the calibration weight arrangements of the known state of the art have relatively large drive mechanisms. However, the known state of the art offers more and more weighing modules containing force-measuring cells which have small dimensions especially in the directions perpendicular to the load vector. These weighing modules are used for measuring small weights that must meet relatively high accuracy requirements. They are also particularly well suited for applications where weighing modules or force-measuring cells are put together in a compound arrangement in systems for production plants, serving to determine the mass of uniform weighing objects as in the checking of small, relatively expensive parts, for example in filling and packaging machines for tablets, capsules, ampoules, etc. in the pharmaceutical industry, or in the quality control of ball bearings.
To make an improvement in the calibration weight arrangement therefore requires in particular an optimization and miniaturization of the drive source for the transfer mechanism. The drive source needs to be very small, compact and flexible to meet different application requirements.
SUMMARY
This task is solved by a force-measuring cell with a calibration weight arrangement and by a weighing device, as claimed in the accompanying claims.
A force-measuring cell is suitably designed for installation in a receiving structure with a plurality of force-measuring cells of the same type. Within the receiving structure each force-measuring cell occupies a design space whose dimensions in a plane that extends orthogonal to the direction of the load are delimited by the design spaces of neighboring force-measuring cells and/or by the largest dimension of the force-measuring cell in said plane. The force-measuring cell comprises parallel-guiding diaphragms arranged, respectively, above and below the force-measuring cell. The force-measuring cell includes a calibration weight arrangement with at least one calibration weight that can be coupled to the force-measuring cell, and it also includes a drive mechanism and a transfer mechanism for the guided movement of the calibration weight. The drive mechanism includes an actuator working together with the transfer mechanism and at least one piezoelectric element driving the actuator. The actuator has at least two elements which interact with each other through the repeated engagement and release of a frictional contact force which occurs during the travel movement in one direction.
An actuator, as the term is used in the present context, encompasses the elements of the drive mechanism which perform a movement, wherein a kinematic behavior of the desired kind and direction often occurs as a result of at least two elements working together.
A calibration weight arrangement which is equipped with a drive mechanism that includes a piezoelectric element has the advantage that only a small amount of space is required to add the drive mechanism to the calibration weight arrangement. The drive mechanism is small and compact and can therefore be placed at any desired location. As a further advantage, the accumulation of electrostatic charges in the drive mechanism or its components is avoided. The drive mechanism further has no magnetic or magnetizable components which could interfere with the operation of a force-measuring cell of a balance that operates according to the principle of electromagnetic force compensation.
The transfer mechanism of the calibration weight arrangement includes a lifting element, a seat for the calibration weight, and a guiding device. This mechanism produces a guided movement, in particular a vertical movement, of the calibration weight seat and thus also of the calibration weight itself, so that when a calibration is taking place, the calibration weight can be brought into force-transmitting contact with the force-transmitting device of the force-measuring cell of a balance. After the calibration has been successfully completed, this force-transmitting contact has to be released again and the transfer mechanism needs to be returned to its rest position. This task is solved through the especially advantageous way in which the drive mechanism works, as the direction of movement is reversible with this kind of drive mechanism, which means that the upward and downward movements are accomplished with the same elements.
This drive mechanism has the further advantage that it is easy to realize a desired velocity profile in controlling the movement of a calibration weight that is to be brought into or returned from its calibrating position by means of the transfer mechanism. It is advantageous if the handing-over of a calibration weight, i.e. that phase where it comes into force-transmitting contact with the force-transmitting device, is performed with the slowest possible speed in order to avoid shocks as much as possible and further to allow the calibration weight to seat itself precisely on the calibration weight carrier that is connected to the force-transmitting mechanism.
As a further distinctive trait, due to the self-locking nature of the drive mechanism, the calibration weight seat which is in most cases movable in the vertical direction is immobilized when there is no current flowing in the drive mechanism.
In an advantageous embodiment of the calibration weight arrangement, the drive mechanism is equipped with a linear piezoelectric motor which has at least one piezoelectric element and a traveler element. The calibration weigh seat can be arranged directly on the traveler element of the linear motor, or the propulsive force of the linear motor can act on the calibration weight seat through an interposed direction-changing element, for example a lever.
According to a further possible embodiment of the calibration weight arrangement, the drive mechanism includes a rotary piezoelectric motor, in particular a traveling wave motor or a motor with a ring-shaped piezo element, which has a shaft on which the lifting element performs a vertical movement by means of a spindle that is an integral part of the shaft.
In a further development of the subject of the invention, the drive mechanism can be equipped to perform a sensor function to monitor the proper functioning of the transfer mechanism. The monitoring of the current for activating the piezoelectric element or of the inductivity of the feedback loop can be used for example to determine the position of the lifting element and the calibration weight.
In a preferred embodiment, the piezoelectric element of the drive mechanism of the calibration weight arrangement has a pusher finger that moves along an elliptical path, wherein the finger in the course of this movement can periodically come into contact, i.e. enter into a frictional or form-fitting engagement, with a drive wheel. A piezoelectric drive of this kind is disclosed for example in WO 01/71899. The pusher finger sets the drive wheel as well as a shaft with an external thread into rotation, while a guide platform with an internal thread is arranged to move along the shaft. However, in performing its elliptical movement, the pusher finger can also act directly on the lifting element or on the calibration weight seat, advancing the latter directly through periodic frictional contact or form-fitting engagement.
Embodiments of the broadest variety are conceivable for the lifting element of a calibration weight arrangement. As an example, the lifting element of the transfer mechanism can be configured as an eccentric or as a pair of wedges that move in opposition to each other. The lifting element of the transfer mechanism can also be realized in the form of at least one knee lever element.
Due to the undesirable heat generation of the drive source, the latter is arranged in a recess in the base plate on which the force-transmitting device is mounted. The base plate can have a reduced thickness in the area of the recess where an opening can be arranged for the passage of at least a part of the lifting element, for example for a shaft which can be constrained by a bearing in the opening. Thus, the excess heat is carried away through the base plate and possibly through the housing.
Due to their small spatial requirements, drive mechanisms containing a piezoelectric element are particularly well suited for use in a calibration weight arrangement of weighing modules, more specifically force-measuring cells of small dimensions primarily in the directions perpendicular to the load. When these drive mechanisms are used in a compound of weighing modules of the same type, they drive the lifting elements in the transfer mechanisms of the respective calibration weight arrangements of individual force-measuring cells. In such a compound, the force-transmitting mechanism of each force-measuring cell is coupled individually to an associated calibration weight. This is particularly useful if not all of the force-measuring cells of the compound system of weighing modules need to be calibrated, but only individual ones among them. A weighing device of this kind has at least two force-measuring cells or weighing modules. However, more typically there are several, for example four, six, eight, nine or even more force-measuring cells arranged in a two-dimensional matrix for the purpose of weighing objects of a uniform nature.
In a particularly advantageous embodiment, the drive mechanism and the transfer mechanism are arranged within the design space below or above the force-measuring cell to which they belong.
In a compound system of weighing modules, a drive mechanism with a piezoelectric element could of course be used to simultaneously couple several calibration weights to the respective force-measuring cells of at least two weighing modules as well as to subsequently uncouple the calibration weights. The compound system of weighing modules contains at least one transfer mechanism and for each weighing module at least one calibration weight which can be coupled to and uncoupled from the calibration weight carrier of the respective weighing module. The at least one transfer mechanism has calibration weight seats that are connected to each other for the respective calibration weights of at least two weighing modules.
Calibration weight arrangements can be realized whereby one or more calibration weights can be coupled to a force-transmitting mechanism by means of a transfer mechanism. An embodiment where a plurality of calibration weights are added one after another to the force-transmitting mechanism and taken off again is especially well suited to determine the linearity.
BRIEF DESCRIPTION OF THE DRAWINGS
The layout of a calibration arrangement in relation to a force-transmitting device of an electronic balance as well as a preferred embodiment of the calibration weight arrangement are shown in the drawings which are described in the following and wherein:
FIG. 1 is a perspective view of a receiving structure with two weighing modules which have parallel-guiding diaphragm springs arranged above and below the force-measuring cell, also indicating the design spaces of the weighing modules;
FIG. 2 is a perspective view of a force-measuring cell of small dimensions perpendicular to the direction of the load, with a calibration weight arrangement for one calibration weight;
FIG. 3 is a perspective view of a force-measuring cell of small dimensions perpendicular to the direction of the load, with a calibration weight arrangement for two calibration weights;
FIG. 4 is a schematic side view of a transfer mechanism with a lifting element configured as a knee-lever element;
FIG. 5 is a schematic side view of a further transfer mechanism with a lifting element configured as a knee-lever element; and
FIG. 6 is a schematic cross-sectional view of an enlarged detail of a base plate in which an actuator is arranged.
DETAILED DESCRIPTION
Due to their small spatial requirements, drive mechanisms containing a piezoelectric element are particularly well suited for use in a calibration weight arrangement of weighing modules that have force-measuring cells with small dimensions in the directions perpendicular to the load. For example in a compound of weighing modules, these drive mechanisms drive the lifting elements in the transfer mechanisms of the respective calibration weight arrangements of individual force-measuring cells. In such a compound, the force-transmitting mechanism of each force-measuring cell is coupled individually to an associated calibration weight. An example for arranging such small-dimensioned force-measuring cells in a compound is illustrated through the embodiment shown in FIG. 1 and described in the following.
In a perspective view, FIG. 1 shows a receiving structure 50 with two weighing modules 51 A, 51 B according to the invention, which form a device for the weighing of objects of a uniform nature. Each weighing module 51 A, 51 B includes, respectively, a force-measuring cell 52 A, 52 B with a load receiver 53 A, 53 B. Each of these weighing modules 51 A, 51 B is arranged within a design space 54 A, 54 B. The dimensions of the respective design space in a plane that is orthogonal to the direction of the load are delimited by the design spaces of adjacent force-measuring cells and/or are equal to the largest dimensions of the force-measuring cell 52 A, 52 B in said plane within the respective design space 54 A, 54 B.
The dimension in the direction of the load is delimited for example by a housing floor which is solidly connected to the receiving structure, or by a base plate 134 . In the direction against the load vector, the design spaces 54 A, 54 B are delimited for example by the tops of the load receivers 53 A, 53 B, for example for the reason that the area above the load receivers 53 A, 53 B is normally occupied by the operating space of a conveyor system which is not shown in the drawing.
The weighing module 51 A is solidly connected to the receiving structure 50 through fastener means 55 , for example screws. The force-measuring cell 52 A of the weighing module 51 A includes a coil, arranged inside the force-measuring cell 52 A and not shown in the drawing, which is connected to a force-transmitting rod 56 A which traverses the force-measuring cell 52 A in the direction of the load. Attached to the upper end of the force-transmitting rod 56 A is the load receiver 53 A.
Arranged between the load receiver 53 A and the force-measuring cell 52 A is an upper parallel-guiding diaphragm 57 A, whose upper parallel-guiding member 58 A connects the upper movable parallel leg 59 A to the upper stationary parallel leg 60 A with a prescribed guiding distance.
Guiding distance, as the term is used here, means the direct distance between the movable parallel leg 59 A and the stationary parallel leg 60 A of the parallel-guiding diaphragm 57 A. With regard to this guiding distance, it is irrelevant how the parallel-guiding member 58 A connecting the two legs is configured.
However, the parallel-guiding member 58 A is shaped so that its effective length is significantly greater than the guiding distance of the parallel-guiding diaphragm 57 A. The effective length is defined as the actual stretched-out length, more specifically the length of the stress-neutral fiber (with regard to bending stress) of the parallel-guiding member 58 A including its connecting areas with the parallel legs 59 A and 60 A.
The upper movable parallel leg 59 A is connected to the force-transmitting rod 56 A, and the upper stationary parallel leg 60 A has a fixed connection to the force-measuring cell 52 A. On the side that faces away from the load receiver 53 A the force-measuring cell 52 A has likewise a lower parallel-guiding diaphragm 61 A whose lower parallel-guiding member 62 A connects the lower movable parallel leg 63 A to the lower stationary parallel leg 64 A, as shown in the break-away drawing of the force-measuring cell 52 A in FIG. 1 . The lower movable parallel leg 63 A is likewise connected to the force-transmitting rod 56 A, and the lower stationary parallel leg 64 A is likewise secured to the force-measuring cell 52 A.
The effective length of the upper parallel-guiding member 58 A should be identical to the effective length of the lower parallel-guiding member 62 A, as it would hardly be possible otherwise to achieve a precisely guided parallel movement of the force-transmitting rod 56 A.
The description of the weighing module 51 A analogously applies to the weighing module 51 A, its upper parallel-guiding diaphragm 57 B and lower parallel-guiding diaphragm 61 B.
For a problem-free exchange of weighing modules 51 A, 51 B arranged side-by-side in a device for the weighing of articles of a uniform nature, no part of a weighing module 51 A that is to be exchanged may protrude beyond the boundaries of its design space 54 A. The movable parallel leg 59 A therefore needs to be arranged within the design space 54 A. In the extreme case, the outside contour of the movable parallel leg 59 A, the parallel-guiding member 58 A or the stationary parallel leg 60 A can be equal to the outside contour of the design space cross-section orthogonal to the direction of the load.
Of course, this arrangement is not limited to two weighing modules 51 A, 51 B. Any number of weighing modules can be arranged behind each other and side-by-side in a two-dimensional layout, wherein any two neighboring force-measuring cells are grouped together in the manner illustrated.
FIG. 2 shows a weighing module with a force-measuring cell 52 of small dimensions, specifically in the projection into a plane that is orthogonal to the direction of the load. A force-measuring cell 52 of this kind can for example have a square profile in the plane that is orthogonal to the direction of the load, measuring a few centimeters along the edges. Of course, round or rectangular profiles are also conceivable. The force-measuring cell 52 in FIG. 2 is illustrated with a calibration weight arrangement 304 specially designed for it. With this calibration weight arrangement 304 it is possible for example in a compound arrangement of force-measuring cells to calibrate each individual force-transmitting device of these force-measuring cells individually. The calibration weight arrangement 304 is distinguished by the fact that a pusher finger 220 moves the lifting element 323 up and down directly by periodically engaging and releasing a frictional contact with a traveling rod 68 which is a part of the lifting element 323 and of the actuator.
The transfer mechanism has a plate-shaped calibration weight seat 314 . The ring-shaped calibration weight 303 is transferred by the transfer mechanism from the rest position to the calibrating position and back again from the calibrating position to the rest position.
Formed on or fastened to the force-transmitting rod 56 A is a calibration weight carrier 102 which in this case is likewise ring-shaped. In the calibrating position as illustrated in FIG. 2 , the calibration weight 303 is in force-transmitting contact with the calibration weight carrier 102 . Ideally, the calibration weight 303 and/or the calibration weight carrier 102 have positioning means whereby the calibration weight 303 is correctly positioned relative to the calibration weight seat 302 and relative to the transfer mechanism.
FIG. 3 illustrates that the calibration weight arrangement described in FIG. 2 is also suitable for the lifting and lowering of two calibration weights 303 A, 303 B. This is particularly useful if linearity errors are to be measured. In making such measurements, it is not necessarily required for the calibration weights 303 A, 303 B to be of equal mass. The calibration weight arrangement of the force-measuring cell 152 has two plate-shaped calibration weight seats 314 A, 314 B. As may be seen in FIG. 3 , the calibration weight 303 B is resting on the calibration weight carrier 102 B and is therefore in calibrating position, while the calibration weight 303 A is in contact with the calibration weight seat 314 A. By lowering the two plate-shaped calibration weight seats 314 A, 314 B farther, the calibration weight 303 A will likewise come into contact with its calibration weight carrier 102 A.
The lifting and lowering of the lifting element 423 is accomplished by the combined action of the piezoelectric drive mechanism which is mounted on the base plate 334 and the traveling rod 168 , wherein the pusher finger 220 forms an actuator which engages the traveling rod 168 with a periodic, or repetitively pulsating, frictional contact force. The direction of movement is reversible with this type of drive mechanism, which means that the upward- and downward movements are accomplished by the same elements.
It should be noted here that, deviating from FIGS. 2 and 3 , the drive mechanism as well as the transfer mechanism could also be arranged below or above the force-measuring cell, within the design space as defined in FIG. 1 . For example, with an embodiment of the force-measuring cell 52 A according to FIG. 1 , the force-transmitting rod 56 A could be extended in the downward direction and equipped with a ring-shaped calibration weight carrier. A likewise ring-shaped calibration weight is, in its calibrating position, in contact with the calibration weight carrier and rests, in its rest position, on a fork-like calibration weight seat which is arranged for example directly on the traveling element of a piezoelectric drive mechanism.
Design configurations of the greatest diversity are conceivable for the lifting element of a calibration weight arrangement. Among these are concepts that are known from the prior art and will therefore only be mentioned in passing here, including arrangements of wedges moving in opposition to each other, or eccentrics on which a calibration weight seat with or without a guide platform is riding. FIGS. 4 and 5 show two further embodiments of lifting elements 123 in the form of different knee lever elements 47 , 147 which are actuated directly by the pusher finger 120 of the drive mechanism containing a piezoelectric element.
FIG. 4 represents in a schematic side view a calibration weight seat 314 which is vertically movable along two guide posts 127 . The lifting element 123 has a disk-shaped knee lever element 47 whose first part 49 is pivotally connected to a leg 48 that is connected to the calibration weight seat 314 . The first part 49 of the knee lever element 47 is likewise pivotally connected to a second part 65 . The latter is connected to a foundation, for example to the base plate 134 , again through a pivotal joint. The second part 65 includes a portion with a semicircular convexity 66 whose outside surface is engaged by a pusher finger 120 of a drive mechanism as described above. This has the effect that the semicircular convexity 66 is moved along the point of engagement of the pusher finger 120 ; the knee lever element 47 straightens or bends, whereby the calibration weight seat 314 is moved in the vertical direction.
In a representation analogous to FIG. 4 , FIG. 5 shows a further embodiment of a knee lever element 47 , where the second part 165 of the knee lever element 147 is configured as a disk-shaped frame with an internal surface profile 67 shaped like a part of a circle. The pusher finger 120 acts on the inside of the frame, and the internal surface profile moves along the point of engagement of the pusher finger 120 , whereby the knee lever element 147 is caused to straighten or bend so that the calibration weight seat 314 is moved in the vertical direction.
Since a drive mechanism with a piezoelectric element generates heat during operation, which is undesirable in the space occupied by the force-measuring cell of a balance, the drive mechanism in an embodiment of the force-measuring cell as shown schematically in FIG. 6 as an enlarged detail of FIG. 1 is installed in a recess 33 of the base plate 34 on which the force-transmitting mechanism is arranged. The part of the base plate 34 which remains between the drive wheel 117 of the actuator and the guide platform 16 has an opening 45 through which the shaft 126 passes. The opening 45 contains a bearing 46 which constrains the shaft 126 . Thus, the excess heat is carried off through the base plate 34 and, if applicable, through a housing that is connected to the base plate. This arrangement has the further advantage that abraded matter which may possibly be produced by the friction between the pusher finger 120 and the drive wheel 117 originates outside of the space containing the force-measuring cell and therefore does not contribute to the contamination of the latter. According to a further variation, the drive mechanism is accommodated in a recess of the base plate which is open from above.
As is self-evident, a multitude of drive mechanisms which include at least one piezoelectric element could be used here. Examples that may be mentioned include a traveling wave motor, an ultrasonic motor with a ring-shaped piezo element, a linear piezoelectric drive, or a so-called caterpillar drive.
Since the drive mechanism with a piezoelectric element is self-locking, which means that when the current is switched off the traveling element is kept immobilized in its current place, the position occupied at that time by the calibration weight seat is secured without requiring any further action.
The drive mechanism can in particular be equipped to perform a sensor function to monitor the proper functioning of the transfer mechanism. The monitoring of the current for activating the piezoelectric element or of the inductivity of the feedback loop can be used for example to determine the position of the lifting element and the calibration weight.
Calibration arrangements of the kind presented herein can be used in balances of high resolution as well as in balances with a lower level of resolution. | A force-measuring cell is designed for a receiving structure having multiple force-measuring cells of the same type. Each cell in the receiving structure occupies a design space whose dimensions, projected into a plane orthogonal to the load direction, is delimited by the design spaces of neighboring and/or is equal to the largest dimension of the cell in the plane. The cell has parallel-guiding diaphragms arranged on upper and lower surfaces thereof. The cell includes a calibration weight arrangement with a calibration weight which can be coupled to the cell, as well as a drive mechanism and a transfer mechanism for guidedly moving the calibration weight. An actuator works together with the transfer mechanism and a piezoelectric element that drives the actuator. The actuator has at least two interacting elements to repeatedly engage and release each other by frictional contact force which occurs during the travel movement in one direction. | 6 |
CROSS REFERENCE TO RELATED APPLICATIONS
Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention is in the field of downhole jarring devices used in oil and gas well drilling and downhole equipment recovery. More specifically, it is a device that imparts rapid impacts to the desired portion of the work string or a stuck object, often referred to as a “fish”, for the purpose of loosening the stuck object.
2. Background Art
In well operation, there is often a need for jarring, impact or vibration devices to move downhole stuck members. Jars are typically included in a pipe or work string to provide upward or downward impacts when activated. Jars are usually single impact devices which must be recocked each time before operation, limiting the number of impacts per minute, and therefore limiting the energy, that can be delivered to a stuck member.
Some known impact tools require the operator to pull up on the work string with a force sufficient to pre-stress the work string, thereby providing the motive force for an impact. The impact is typically initiated when some type of valve or other triggering device in the tool triggers an action which applies the energy stored in the pre-stressed work string in the form of an impact delivered to the stuck object. The force of the impact delivered by such a tool depends upon how much energy is stored in the pre-stressed work string. That is, a larger over-pull will deliver a harder blow to the stuck object.
Often, in the use of this type of tool, the weight of the fish itself can be significant enough to raise the tension in the work string to such a high level that the tool will cease to function. More specifically, the force which can be applied to the triggering device by the flow of fluid is limited by the available fluid flow rate. The higher the amount of pre-stress tension, the harder it is to make the tool function. If the weight of the fish is too close to the pre-stress limit of the tool, the tool will cease to function as the fish begins to loosen. The operator then has to reduce the pre-stress on the work string to make the tool resume functioning, thereby limiting the force available in each impact and making the tool less effective.
Further, a tool which relies on work string pre-stress often has a fluid flow path which allows well bore return fluid to enter the tool, which exposes the internal tool parts to well bore debris. This can clog or restrict the moving parts and render the tool inoperative, it can cause failure of the seals, or it can cause the tool to wear out prematurely.
BRIEF SUMMARY OF THE INVENTION
The device of the present invention uses hydraulic power from surface pumps to repeatedly compress an internal piston spring in the tool. The piston spring is repeatedly allowed to expand, to deliver continuous rapid impacts. The sustained energy that is delivered to the stuck member becomes a motivating force to free the stuck member. When the operator desires, the fluid flow rate through the tool is increased to a selected level, which will exert sufficient hydraulic pressure to move a dart valve to seal against a valve seat on a flow-through piston. This cuts off flow through the piston and drives the piston and the dart valve downwardly. As the piston moves downwardly, it compresses the piston spring. At a designed tripping point, the dart valve is lifted away from the valve seat on the piston by a tripping spring, allowing flow through the piston to resume, sharply decreasing the hydraulic pressure on the piston. This allows the piston spring to drive the piston sharply upward, delivering an impact to the tool housing. Movement of the dart valve away from the piston seat is arrested by a momentary increase in hydraulic pressure above the dart valve, caused by a momentary cutoff of fluid flow through the dart valve. The dart valve is then driven downwardly again, and the cycle repeats rapidly.
The motive force for the impact is generated entirely within the tool, eliminating any need for prestressing the tool from above. This allows the tool to function regardless of the weight of the stuck object. No return fluid flow passes through the tool, eliminating the danger of contamination by well debris.
The novel features of this invention, as well as the invention itself, will be best understood from the attached drawings, taken along with the following description, in which similar reference characters refer to similar parts, and in which:
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
FIG. 1 is a longitudinal quarter section view of the tool of the present invention;
FIG. 2 is a partial section view of the tool shown in FIG. 1, prior to movement of the dart valve;
FIG. 3 is a partial section view of the tool shown in FIG. 1, after movement of the dart valve to seal against the valve seat on the piston;
FIG. 4 is a partial section view of the tool shown in FIG. 1, after further downward movement of the dart valve and the piston to compress the dart valve spring and the piston spring; and
FIG. 5 is a partial section view of the tool shown in FIG. 1, after separation of the dart valve from the valve seat, and after upward movement of the piston to impact the housing.
DETAILED DESCRIPTION OF THE INVENTION
The vibratory tool 10 of the present invention is shown in quarter section in FIG. 1 . It is comprised of an outer housing assembly made up of a top sub 12 , a shoulder stop 14 , a clutch 16 , a clutch housing 18 , a piston housing 20 , and a bottom sub 22 . The outer housing assembly provides means of transmitting tension and torque through the tool 10 . As tension is applied at the top sub 12 , it is transmitted to the clutch 16 through connecting threads. The clutch 16 is free to travel axially on the clutch housing 18 . The clutch 16 contains one or more seals 24 which prevent communication of fluid from the interior of the tool 10 to the exterior of the tool 10 during axial movement of the clutch 16 . Upward axial travel of the clutch 16 is limited by shouldering up against the shoulder stop 14 , which is threaded tightly against the clutch housing 18 . The shoulder stop 14 is prevented from backing off during operation of the tool 10 by one or more set screws 26 . Axial tension is passed from the clutch 16 , through the shoulder stop 14 , then to the clutch housing 18 , the piston housing 20 , and the bottom sub 22 .
Torque applied through the top sub 12 is transmitted through threads to the clutch 16 . The clutch 16 transmits torque to the clutch housing 18 through meshed fingers on both the clutch 16 and the clutch housing 18 . Torque is transmitted from the clutch housing 18 to the piston housing 20 and the bottom sub 22 via threaded connections. The outer housing assembly is sealed by a plurality of seals 24 , 28 , 30 , and 32 .
The fingered slip joint between the clutch 16 and the clutch housing 18 isolates the top sub 12 and the shoulder stop 14 from longitudinal impacts traveling upward through the clutch housing 18 , and reflects longitudinal shock waves back down through the clutch housing 18 , the piston housing 20 , and the bottom sub 22 , to the lower portion of the string or to the fish, not shown.
One or more upper and lower piston springs 34 , 36 bias a piston 38 upwardly. The upper and lower piston springs 34 , 36 are initially preloaded to give a selected upward biasing force against the piston 38 . The two lower piston springs 36 are separated by a lower piston spring retainer 40 , containing a wear guide 42 . The spring force from the lower piston springs 36 is transmitted to a mandrel 44 through a lower piston spring stop 46 , containing another wear guide 42 . The mandrel 44 is threaded into the bottom portion of the piston 38 to transmit the spring force from the lower piston springs 36 to the piston 38 . The mandrel 44 also serves as a guide to the upper piston springs 34 . One or more set screws 47 serve to help retain the mandrel 44 to the piston 38 .
A sleeve 48 and an upper piston spring stop 50 act to isolate the spring forces of the upper piston springs 34 , so they can transmit spring forces directly to the piston 38 , independently of the lower piston springs 36 . The two upper piston springs 34 are separated by an upper piston spring retainer 52 , containing a wear guide 54 . The piston 38 is free to move axially inside the piston housing 20 and the clutch housing 18 . The piston 38 is centralized by at least two wear guides 56 , 58 . Piston rings 60 provide dynamic sealing between the piston 38 and the clutch housing 18 .
An impact ring 62 separates the piston 38 from the clutch housing 18 and restricts the upward axial movement of the piston 38 . Importantly, when the piston 38 moves upwardly, the impact ring 62 also distributes impact forces from the piston 38 to the clutch housing 18 .
The piston 38 is hollow, to allow fluid flow therethrough. Contained within the upper end of the piston 38 is an annular valve seat 64 . The valve seat 64 is retained to the piston 38 by at least one set screw 66 which lies beneath the upper piston ring 60 , to prevent backing off of the set screws 66 . The valve seat 64 is sealed inside the piston 38 by two seals 68 .
Inside the clutch housing 18 is a dart valve mechanism comprising a sleeve retainer 70 , a dart valve sleeve 72 , and a dart valve body 74 . The sleeve retainer 70 has holes therethrough, and the dart valve body 74 is hollow, to allow fluid flow therethrough. Surrounding the dart valve body 74 is a valve spring assembly made up of a spring stop 76 , a valve trip spring 78 , a standoff sleeve 80 , a standoff spring 82 , and a dart valve guide 84 . The dart valve guide 84 is held in place by an o-ring 86 . The spacing of the valve spring assembly is such that the valve spring assembly and the dart valve body 74 are free to travel axially.
The standoff spring 82 is weaker than the valve trip spring 78 , and the standoff spring 82 is spaced so that the dart valve body 74 , the spring stop 76 , and the valve trip spring 78 can be allowed an initial shift in the downward axial direction without compressing the valve trip spring 78 . This initial downward shift allows the dart valve body 74 to seal against the valve seat 64 in the upper end of the piston 38 , stopping fluid flow through the piston 38 . The standoff sleeve 80 prevents overtravel of the valve spring assembly in the downward axial direction. Upward movement of the valve spring assembly is stopped by abutment of the spring stop 76 against the dart valve sleeve 72 . The dart valve body 74 is concentrically located within the valve spring assembly, the standoff sleeve 80 , and the dart valve guide 84 .
After the standoff sleeve 80 contacts the dart valve guide 84 , a shoulder on the upper end of the dart valve body 74 seats against the spring stop 76 , so that as the dart valve body 74 travels downwardly, the valve trip spring 78 is compressed. Downward axial travel of the dart valve body 74 is limited by abutment of the spring stop 76 with an annular internal shoulder 88 on the clutch housing 18 .
Operation of the tool 10 is illustrated in FIGS. 2 through 5. FIG. 2 shows a close up of the tool 10 in the configuration in which it is run into the well bore. The standoff spring 82 provides an initial biasing of the dart valve body 74 toward an open position, spacing the dart valve body 74 away from the piston valve seat 64 , allowing flow through the tool. When the fluid flow rate is selectively increased by the operator to a critical flow rate, the increased fluid resistance of the dart valve body 74 causes the dart valve body 74 to move downwardly, compressing the standoff spring 82 , until the standoff sleeve 80 contacts the dart valve guide 84 , and the dart valve body 74 comes into contact with the valve seat 64 , as shown in FIG. 3 . At this point, the fluid flow through the tool 10 is shut off, and pressure begins to build against the upper end of the piston 38 and the dart valve body 74 .
This increased fluid pressure pushes the piston 38 downwardly, compressing the upper and lower piston springs 34 , 36 , as shown in FIG. 4 . As the dart valve body 74 moves downwardly with the piston 38 , the dart valve trip spring 78 is also compressed, providing an increasing upward force against the dart valve body 74 . At the point where the downward hydraulic pressure force on the dart valve body 74 equals the upward force created by the dart valve trip spring 78 , the dart valve body 74 separates from the valve seat 64 , and the valve spring assembly suddenly retracts away from the piston 38 , as shown in FIG. 5 .
The upward momentum of the valve spring assembly and the dart valve body 74 is used to temporarily shut off fluid flow through the dart valve body 74 , to stop the valve spring assembly and the dart valve body 74 from overtravel in the upward direction. This is accomplished by restricting the fluid that can bypass the valve spring assembly. As the dart valve body 74 moves upwardly, the flow passage through the dart valve body 74 is gradually restricted as the flow path through the outside diameter of the dart valve body 74 is shut off by the inner diameter of the dart valve guide 84 . As the flow becomes restricted, pressure is built up above the dart valve body 74 , slowing the dart valve body 74 , the dart valve trip spring 78 , the standoff sleeve 80 , and the standoff spring 82 , until the upward travel of the dart valve body 74 and the valve spring assembly is halted. The pressure then returns the dart valve body 74 and the valve spring assembly to its operating position.
As the dart valve body 74 moves upwardly, the seal between the dart valve body 74 and the valve seat 64 is lost, causing a rapid drop in pressure above the piston 38 . Since the downward hydraulic pressure force is lost, the upper and lower piston springs 34 , 36 cause the piston 38 to rapidly return and strike against the impact ring 62 , causing a sharp upward impact to be delivered to the clutch housing 18 , as shown in FIG. 5 . The dart valve body 74 then reseats on the valve seat 64 , and the entire cycle repeats numerous times each second. This process continues for as long as a sufficiently high rate of fluid flow is maintained through the tool 10 by the operator.
While the particular invention as herein shown and disclosed in detail is fully capable of obtaining the objects and providing the advantages hereinbefore stated, it is to be understood that this disclosure is merely illustrative of the presently preferred embodiments of the invention and that no limitations are intended other than as described in the appended claims. | A vibratory impact tool for loosening downhole stuck objects in oil or gas wells, utilizing an internal piston spring which is repeatedly compressed by hydraulic pressure, and repeatedly released by lifting a dart valve from a valve seat on a flow-through piston. When the dart valve is lifted from the valve seat by a tripping spring, flow resumes through the piston, quickly lowering hydraulic pressure above the piston, allowing the piston spring to sharply drive the piston against the housing. The dart valve is then reseated on the valve seat, causing the piston to again be driven against the piston spring, rapidly repeating the process. | 4 |
FIELD OF THE INVENTION
The invention relates to a yarn feeding device and more specifically to the use of an electric synchronous motor for controlling a yarn feeding device.
BACKGROUND OF THE INVENTION
The yarn feeding device known from EP 0 580 267 A1 comprises a pre-control device using the signals of a position sensor provided in the yarn feeding device in order to slowly drive the electric motor after switching off the electric motor by the speed control device until the winding element reaches a predetermined rotational position in relation to the housing. The control effort needed is considerable.
The yarn feeding device as known from EP 0 327 973 A (U.S. Pat. No. 4,936,356) is provided with a detector fixed to the housing which detector can be actuated by a transmitter rotating with the winding element in order to adjust the winding element with slow rotational speed into a predetermined position relative to the housing when the speed control device has to switch off the electric motor. The predetermined position of the winding element may be appropriate in order to facilitate threading of the yarn through the yarn feeding device.
U.S. Pat. No. 4,814,677 A generally discloses a field orientation control system of a permanent magnet motor operating by sinusoidal stator part actuation. The information on the momentary rotary position of the rotor is derived from measured stator voltages and stator currents. This is carried out without additional position sensors. The detected relative rotary positions of the rotor are used for the speed control and the torque control of the permanent magnet motor.
The so-called brushless DC motor (BLDC) known from EP 10 52 766 A2 (U.S. Pat. No. 6,356,048) is employed as the drive source for the winding element of a yarn feeding device. The motor is designed without sensors. A control system is provided for controlling the torque and/or the speed of the motor. The control system calculates the commutation switching points for the stator parts in six angled positions which are distant by a respective 60° without a position sensor. In this case the zero crossing points of the backwards acting electromotive force are determined which are induced in the stator windings by the rotation of the rotor magnets. In-between the six switching points, distributed about a full revolution, the position of the rotor remains unknown. The backwards acting electromotive force is effected according to a trapezoidal course. This motor drive control principle does not allow a sufficiently accurate position control and position observation of the winding element because only predetermined rotary positions of the rotor are detected.
SUMMARY OF THE INVENTION
It is an object of the invention to provide a yarn feeding device of the kind as disclosed herein which allows in a structurally simple and controllable fashion an accurate position control and/or position observation of the winding element in order to selectively and precisely reproducibly adjust a predetermined rotary position of the winding element which rotary position is needed for an auxiliary function of the yarn feeding device.
Additionally, this object can be achieved particularly expediently and simply by employing an electric synchronous motor for the control of the yarn feeding device, particularly a permanent magnet motor, which operates with permanent (continuous) stator vector control and sinusoidal stator actuation, in order to carry out the position control and/or position observation of the winding element in relation to the housing of the yarn feeding device, and to use for that purpose the information about the respective rotary position of the rotor which anyhow is needed for the permanent (continuous) stator vector control.
The speed device equipped with the microprocessor detects permanently (continuously) the relative rotary position of the vector of the rotor which position corresponds to the momentary rotary position of the rotor. This is carried out to permanently (continuously) rotate the stator vector generated by the sinusoidal actuation of the stator part such that the desired speed and/or the desired torque is gained substantially steplessly. The information on the momentary rotary position of the rotor or the rotor vector, respectively, is used to adjust the winding element into the at least one predetermined relative position in the housing by using the fixed structural correlation between the rotor, the shaft and the winding element. This relative position is useful to thread the yarn by means of an automatic threading device without further checking the rotary position of the winding element, or to adjust the winding element into a position in which a manual threading process can be carried out without problems. Additionally or alternatively, the information by which during the permanent vector control of the rotor rotation is followed can be used to measure the wound on yarn length. The capacity of the microprocessor is sufficient without problems for this additional function. No sophisticated additional control circuits are needed, and also no costly sensor assemblies.
The motor, expediently, is a permanent magnet motor which is available for fair costs and is efficient and takes up only minimal mounting space. Basically, however, also other types of synchronous motors may be used within the scope of this invention, like so-called reluctance motors, so even so-called “switched reluctance motors (SR)”. In principle, even a so-called BLDC (brushless DC motor) could co-operate with the speed control device according to the invention.
In order to be able to permanently (continuously) and precisely follow the movement of the rotor, it is of advantage when the permanent magnets in the rotor are designed (e.g. formed), magnetised and/or configured (placed) such that the backward acting electromotive force induced by the rotor in the stator winding follows a sinusoidal course. With the help of the sinusoidal course the respective rotor rotary position can be calculated accurately which is of advantage for the permanent (continuous) vector control, and which is very suitable as a side product also for the position control and/or position observation of the winding element relative to the housing.
A calculating circuit is, expediently, contained in the speed control device, preferably in a microprocessor, which calculates the relative rotor rotary position with the help of the induced backwards oriented electromotive force. The electromotive force can be measured precisely in terms of its course and its magnitude.
Additionally, if expedient, at least one rotary position sensor may be provided and connected to the speed control device. The signal of this sensor may be used in order to build up a holding torque by means of the motor control and to retain the winding element at the predetermined rotary position relative to the housing despite an externally acting rotary force, and in order to retrieve the rotary position of the winding element or the rotor, respectively, during a restart of the motor.
Expediently, several relative rotary positions of the winding element within a 360° rotation of the winding element are programmed and can be selectively adjusted for correspondingly control stopping of the motor. That means that the winding element as well is stopped in the most suitable rotary position depending on the planned auxiliary function at the yarn feeding device. This relative rotary position can be selected completely arbitrarily.
It is expedient to place the stator part in a predetermined rotary position in the housing. By this measure each desired relative position of the winding element, as programmed, can be set in relation to the housing already during assembly of the yarn feeding device, without the necessity to carry out further programming.
By means of the determined permanent relative rotary position of the rotor during the vector control even the rotary travel of the winding element at least from the start to the end of a driving period can be measured without additional equipment parts, which is useful to precisely measure the wound on yarn length.
Alternatively, the yarn length may be measured in the same fashion even between selected points in time or selected different relative rotary positions of the rotor, respectively, by evaluating the information about the momentary rotor rotation angle for this additional function.
A predetermined relative rotary position of the winding element in relation to the housing may be a full yarn threading position in which an exit opening of the winding element is aligned with a threading path provided in the housing of the yarn feeding device. The on-board pneumatic threading device then may thread a new yarn without further interference by an operator.
Alternatively, the predetermined rotary position of the winding element in relation to the housing and adjustment by means of the vector control may be a semi-threading position in which an exit opening of the winding element is positioned outside of shielding housing parts such that no obstacles hinder the manual gripping of the yarn for knotting the yarn to yarn material already provided on the storage surface, or such that the winding element does not have to be rotated manually into a position beneficial to this auxiliary function.
An electronic yarn length measuring device can be supplied with the information on the rotor rotary positions during the vector control in order to derive precise information on the yarn consumption.
In the case that additionally a position sensor for the winding element is provided in the yarn feeding device, in order to signal at least one position or to confirm a position, respectively, then this position sensor may be used for generating an aligning holding torque by means of the motor and in co-action with the speed control device. The holding torque retains the winding elements in the adjusted rotor position even if external forces tend to further rotate the winding element. The motor control is apt to adapt automatically to the magnitude of the acting external force in order to hold the winding element stationary.
Expediently, the position sensor comprises permanent magnets distributed along the circumference of the winding element, and at least one detecting element fixed to the housing which responds to the passage of each permanent magnet. Preferably, a digitally operating Hall element is provided generating a digital signal whenever a permanent magnet is passing. However, particularly expedient is also an analog Hall sensor responding respectively to one pair of adjacent permanent magnets in order to precisely monitor even rotation ranges of the winding element.
BRIEF DESCRIPTION OF THE DRAWINGS
An embodiment of the invention will be explained with reference to the drawings wherein:
FIG. 1 is a longitudinal section of a yarn feeding device comprising a synchronous electric motor of a permanent magnet type as a driving source for a winding element, and
FIG. 2 is a cross-section of the yarn feeding device.
DETAILED DESCRIPTION
A yarn feeding device F as shown in FIG. 1 and FIG. 2 is a weft yarn feeding device for a weaving machine (not shown). However, the invention can be applied to a yarn feeding device for a knitting machine (not shown) as well, the yarn feeding device then having a rotary yarn storage drum defining a winding element.
The yarn feeding device F in FIGS. 1 and 2 comprises a housing 1 with a housing bracket 2 containing additional components. A hollow shaft 3 is rotatably supported in a bearing 4 in the housing 1 . The shaft 3 stationarily supports by its free end a storage drum D which is positioned below the housing bracket 2 . In order to prevent that the storage drum D from rotating together with the shaft 3 permanent magnets 12 are provided in the housing which magnetically co-act with not shown permanent magnets placed in the storage drum D.
A rotor R is provided on the shaft 3 . The rotor co-acts with stator part S stationarily placed in the housing. The stator S is fixed by a positioning means 13 ( FIGS. 1 and 2 ) in a predetermined rotary position.
An electric motor control device CU containing a microprocessor MP is contained in the housing bracket 2 . The motor control device CU is connected for signal transmission to a yarn sensor assembly 8 and controls the speed, the torque and the rest periods of the electric motor M depending on the size of a yarn store formed by yarn windings on the storage drum D. Furthermore, a yarn threading path 9 is provided in the housing bracket 2 for co-action with a not shown, on-board pneumatic threading device in order to thread a new yarn entirely through the yarn feeding device. Furthermore, a withdrawal opening 7 for the yarn is placed at the housing bracket 2 .
A winding element W having an exit opening 6 is fixed to the shaft 3 . The relative rotary position of the exit opening with respect to the rotor R is structurally fixed. The winding element W may be formed as a funnel-shaped disk 10 containing a not shown winding tube terminating at the exit opening 6 . At the winding element W permanent magnets 11 may be provided which are distributed along the circumference and which co-act with a detecting element H (for example, a digital or analog Hall sensor) stationarily provided in the housing bracket 2 .
The electric motor M is an electric synchronous motor, preferably a permanent magnet motor (a so-called PM-motor). FIG. 2 illustrates the geometric distribution of permanent magnets PM in the rotor R and a schematic view of the stator part S (without stator windings provided therein).
With the help of the speed control device CU and the microprocessor MP a permanent vector control of the motor M is carried out, i.e., the rotary position of the rotor vector is determined continuously without sensors, and the stator vector is rotated by a corresponding current actuation continuously such that the desired speed and an optimum development of the torque result. The actuation of the stator windings is carried out sinusoidally. The permanent magnets PM in the rotor R are designed (formed), magnetised and/or configured (placed) such that, furthermore, forced by the function, the backwards oriented electromotive force in the stator windings resulting from the rotation of the rotor R in relation to the stator parts S will be induced with a sinusoidal course. With the help of the sinusoidal course of the induced electromotive force the rotary position of the rotor vector is continuously determined. The stator vector is rotated according to the determination by actuation of the stator part. The information about the momentary rotary position of the rotor vector or the rotor, respectively, in relation to the stator windings or the stator part S, respectively, and the housing, furthermore is used for the position control and/or the position observation of the winding element W.
Referring to FIG. 2 a predetermined rotary position X 1 of the winding element W is a so-called full threading position in relation to the housing 1 . In this full threading position the exit opening 6 of the winding element W is precisely aligned with the threading path 9 structurally integrated into the housing bracket 2 . In this predetermined rotary position X 1 the yarn while blown through the shaft 3 and out of the exit opening 6 is guided along the threading path 9 and finally is brought into the exit opening 7 without manual interference. However, a prerequisite for this function is that the winding element is stopped precisely at the predetermined rotary position X 1 when the electric motor M is stopped. For adjusting this rotary position X 1 now the permanently (continuously) present information on the rotary position of the rotor R in relation to the stator parts S or the housing, respectively, is used to precisely stop the winding element W at the predetermined rotary position X 1 by means of the speed control device CU, which is useful in the event of a yarn breakage, as detected by not shown detectors.
In FIG. 2 , furthermore, a further predetermined rotary position X 2 is shown for the exit opening 6 of the winding element W. The rotary position X 2 is predetermined such that the exit opening 6 is stopped offset by 90° in relation to the housing bracket 2 , i.e. that the exit opening is not covered by any housing components hindering direct access.
In case that a not shown yarn detector detects a yarn breakage situation while yarn material is still present on the storage surface of the storage drum D, the winding element will be stopped in the rotary position X 2 by means of the vector control of the electric motor M such that the then activated pneumatic threading device will present the blown-through yarn at an easily accessible position of the housing for being gripped by the operator. By a corresponding re-correlation of the signal generated by the yarn detectors the speed control device CU will have been informed beforehand in which of the two predetermined positions X 1 , X 2 the yarn winding element W has to be adjusted for a certain operating condition.
The rotary position sensor H does not need to be used for this task. However, this sensor may assist in preventing undesired rotation of the winding element W when stopped at the respective position X 1 or X 2 , respectively. This means that then the speed control device CU will build a holding torque in the one or the other sense of rotation in order to locally retain the winding element despite the influence of external forces (the yarn tension or the like). Furthermore, the rotary position sensor H may be used for determining the rotary position of the rotor R and at the same time of the winding element W in case of a new operation start-up and as rapidly as possible.
Furthermore, a yarn length measuring device can be interlinked with the speed control device CU in order to measure the length of the wound on yarn by means of the rotary travel Y of the winding element W.
The respective predetermined rotary position X 1 , X 2 may be selected and adjusted arbitrarily, because the control permanently follows the movement of the rotor during operation of the motor and since the respective position information is present continuously. This means that neither the rotary positions X 1 , X 2 , nor further rotary positions of the winding element W as needed for other purposes have to be fixed beforehand either by the geometric relations between the stator S and the rotor R or by the geometric placement of the position sensor H. To the contrary any rotary positions can be freely adjusted or programmed, respectively, as they are best for the auxiliary functions of the yarn feeding device, e.g. for threading processes. The predetermined position X 2 may be varied later by corresponding reprogramming, which is useful in a situation such as where several yarn feeding devices have to be placed close to each other at a weaving machine such that they might block the respective access to the position X 2 in FIG. 2 . In such a case the position X 2 can be put to another location where comfortable access is possible for the operator despite the restriction by the several closely arranged yarn feeding devices.
Although a particular preferred embodiment of the invention has been disclosed in detail for illustrative purposes, it will be recognized that variations or modifications of the disclosed apparatus, including the rearrangement of parts, lie within the scope of the present invention. | The invention relates to a yarn feeding device (F) for weaving or knitting machines whose winding element (W) is driven by an electric motor (M) controlled by an electronic speed control device (CU). According to the invention, the electric motor (M) is a synchronous motor, in particular, a permanent magnet (PM) motor with the speed control device (CU) provided for effecting a permanent vector control with the stator being sinusoidally acted upon. Continuously determined information pertaining to the relevant rotational position of the rotor (R) of the motor (M) is used in the speed control device (CU), which serves to perform permanent vector control, in order to adjust at least one predetermined rotational position (X 1 , X 2 ) of the winding element (W). | 3 |
CROSS-REFERENCE TO RELATED APPLICATION
Not applicable.
STATEMENT OF FEDERALLY SPONSORED RESEARCH/DEVELOPMENT
Not applicable.
BACKGROUND OF THE INVENTION
The present invention relates to shower enclosures and the like. More specifically it relates to support structures provided near corners of such enclosures, and seats for use therewith.
There are occasions when almost any bather may want to be able to sit at normal chair height in a shower enclosure (e.g. to wash feet). Also, the elderly, the handicapped, and certain children often need or desire to be able to sit at normal chair height when showering.
While the largest shower enclosures can provide enough room to install integral (or permanently affixed) seat structures (see e.g. U.S. Pat. No. 6,301,725), some shower enclosures are 48 inches wide or less. For these, it may be undesirable to take up so much room with seats that will always jut out into the standing space. Thus, some enclosures are provided with fold-up seats. However, these types of seats require additional construction and assembly, and risk additional leakage points along the attachment holes.
In connection with bathtubs there have been a variety of removable seats provided that are suspended on opposed front and back walls of the tub. When the bather wishes to sit all the way in the tub, the seat is simply removed. However, this requires there to be a front wall opposed to the rear wall.
For more conventional shower enclosures which do not have a raised front wall, it is more conventional to use the approach of attaching corner seats with fasteners. See U.S. Pat. Nos. 5,542,218 and 5,732,421.
Yet another approach is that of U.S. Pat. No. 3,193,848 which describes a self-standing stool with legs that permit it to be positioned at a corner and temporarily coupled to the corner with suction cups. However, this is not a secure attachment system.
There have also been suggestions to provide a shower enclosure that has at both its left and its right corners pedestals that can be used to somewhat support a removable seat. However, this system did not securely attach the seat without fasteners in situations where most of the weight is at the front of the seat.
Thus, a need still exists for the development of a removable shower seat which can be easily positioned in or removed from a shower module without the use of fasteners, yet which is securely supported.
BRIEF SUMMARY OF THE INVENTION
The present invention provides a combined bathing enclosure and removable seat. The bathing enclosure has (i) a rear wall, (ii) opposed side walls, (iii) a support positioned adjacent a corner of the enclosure, where the corner is defined by a junction between the rear wall and a specified one of said side walls, (iv) a first pocket along the rear wall adjacent the support, and (v) a second pocket along the specified side wall adjacent the support. For purposes of this application, the term “bathing enclosure” is intended to cover any enclosure suitable for bathing, regardless of whether fully enclosed (e.g. a three-sided structure), and regardless of whether having a bathtub for also permitting reclined bathing (e.g. a shower enclosure). There is also a seat removably supportable adjacent the corner with one end of the seat positionable in the first pocket and an opposite end of the seat positionable in the second pocket.
In preferred forms at least one of the pockets has a downwardly sloped surface, and the seat has a surface that can rest on that sloped surface. The rear wall of the enclosure has a ledge adjacent the first pocket opposite the support, and the seat has a flange suitable to rest on that ledge. Also, the specified side wall of the enclosure can have a ledge adjacent the second pocket opposite the support, and the seat can have a wall suitable to rest on that ledge.
Further, the seat can have on its top surface a front edge, a left edge, a right edge, and a rear edge, with the left and right edges being essentially perpendicular to each other. In yet other forms the seat is formed of a base material that is at least partially coated with an elastomer along surfaces that can contact the bathing enclosure when the seat is installed therein.
In accordance with the present invention, the seat can be installed without fasteners, and thus can be removed without marring the shower stall, for cleaning, for when a user wishes to use the shower without a seat, and for when the seat is to be moved to the opposite corner.
The seat is supported on three sides, and on its opposite ends is also supported in angled pockets. Thus, the seat can support substantial weight without tipping, even though it is not bolted to the wall or supported along the front wall.
These and other advantages of the present invention will be apparent from the description that follows. The claims should be looked to in order to judge the full scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is left, frontal, upper perspective of part of a shower enclosure having a seat structure constructed in accordance with the present invention;
FIG. 2 is a top plan view of the seat of FIG. 1;
FIG. 3 is a bottom plan view of the seat of FIG. 2;
FIG. 4 is a front elevational view of the seat of FIG. 2;
FIG. 5 is a rear elevational view of the seat of FIG. 2;
FIG. 6 is a right side view of the seat of FIG. 2;
FIG. 7 is a view similar to FIG. 1, but showing somewhat more of the shower module, and showing the seat in an installed position;
FIG. 8 is a top plan view of a part of the FIG. 7 assembly;
FIG. 9 is a sectional view taken along line 9 — 9 of FIG. 8;
FIG. 10 is a sectional view taken along line 10 — 10 of FIG. 8;
FIG. 11 is a sectional view taken along line 11 — 11 of FIG. 8;
FIG. 12 is a sectional view taken along line 12 — 12 of FIG. 8;
FIG. 13 is a sectional view taken along line 13 — 13 of FIG. 8; and
FIG. 14 is a sectional view taken along line 14 — 14 of FIG. 8 .
DETAILED DESCRIPTION OF THE INVENTION
A removable shower seat 10 that is constructed in accordance with the present invention is shown in FIG. 1 in the process of being installed in a shower enclosure module 28 . The shower seat 10 preferably has a planar top 11 that is contoured trapezoidal. The top is supported by a base section 22 which is sized and dimensioned to be wedged against and into pockets 36 and 38 of the module 28 , as described more fully below.
Referring now to FIG. 2, the seat has right and left side edges 12 and 14 , a front edge 16 , and a rear edge 18 . The right and left side edges 12 and 14 are directed in planes substantially perpendicular to each other. The front edge 16 and back edge 18 extend between the side walls 12 and 14 substantially parallel to each other. Preferably, the front and back edges 16 and 18 are curved, as shown.
The base section 22 has left and right side walls 21 and 23 , respectively, a front wall 25 , and a rear wall 27 . The walls 21 , 23 , 25 , and 27 extend downward in direction substantially perpendicular to a horizontal plane defined by the seat top 11 . The front wall 25 and front edge 16 are generally co-extensive, while the side wall 12 , side wall 14 , and back side wall 18 are offset from the corresponding surfaces of the seat to define a horizontally-extending flange. See also FIGS. 4-6.
Referring now to FIG. 3, it can also be seen that the width of the flange 20 is varied to provide a wider contact surface in defined mounting locations. In particular, the side walls 21 and 23 are angled as they approach the front wall 25 , thereby providing corner mounting sections 29 and 31 , respectfully, at the intersection of the front and side walls.
Referring again to FIGS. 4-6, and FIG. 1, the side walls 21 and 23 are angled to mate with the angled pocket side walls ( 36 and 38 ) of the shower stall, as described more fully below. The walls 21 and 23 are angled upward from the back to the front of the seat 10 . The side walls 21 and 23 are therefore highest at the intersection with the back wall 27 and lowest at the intersection with the front wall 25 .
The back wall 27 has a back support which is formed to mate against the corner wall of the shower stall 28 . However, a small water passage groove 33 is formed in the wall 27 to allow water to drain from both the seat 10 and the supporting region 32 . The water passage area comprises an indentation 33 in the back wall 27 , which operates in a conjunction with a downwardly sloping ridge 35 formed in the seat 11 to direct water.
The seat element 11 and base section 22 are preferably molded as a single piece from a relatively rigid plastic such as polypropylene material. To further provide rigidity, the base section 22 is provided with internal structural ribs.
In accordance with the present invention, a low durometer elastomer material 44 is molded onto contact surfaces along the seat 10 , such as the lower side of flange 20 and the corresponding walls 21 , 23 , and 27 . The plastic material can be polypropylene, preferably a homopolymer having a tensile strength of 4900 psi (ASTM D638) and a flexural modulus of 190,000 psi (ASTM D790). The elastomer is preferably rated at 55±5 durometer. An elastomer of this type is the Santoprene® 8211-55 series available from Advanced Elastomer Systems of Akron, Ohio.
It will be particularly appreciated that the flexibility of the surface should be greater than the flexibility of the shower module walls. This will assist in avoiding having the seat scratch the wall surfaces. The flexible material will also help securely wedge the seat in place.
Referring now to FIGS. 1 and 7, the shower stall module 28 has pockets 36 and 38 . There is also a corner pedestal 32 above a support 40 . A similar construction is provided at the left rear corner of the shower stall to provide the opportunity for the seat to alternatively be mounted at that corner. The pockets have outwardly and downwardly sloping side walls, and opposed end walls. Along the rear wall of the module is a ledge 34 , and along the side wall of the module is a ledge 37 .
As the seat 10 is installed, the portion of the flange 20 extending horizontally from the back wall 27 of the base 22 is received on the corner pedestal 32 . See also FIG. 9 .
The corner mounting portions 29 and 31 of the flange 20 rest on the ledges 37 and 34 . See e.g. FIG. 14 . When this is achieved, both the bottom of the side walls 21 and 23 and the flange section 20 along the side walls 21 and 23 rest against the angled pocket wall sections 36 and 38 , respectively. See FIG. 13 . Because of all of these points of support, the seat can support a wide range of body sizes without tipping.
As noted above, all surfaces which will contact the shower stall 28 are coated with an elastomer material 44 . Apart from the advantages noted above, the elastomer compresses with applied weight, thereby allowing some flex, thereby making seating more comfortable.
Referring next specifically to FIGS. 9-11, detailed views of the back portion of the flange 20 resting on the corner pedestal 32 are shown. Note that the back wall 27 rests along the support section 40 .
Referring next to FIGS. 12 and 13, both the bottom edges of the side walls 21 and 23 and the edge of the flange 20 rests against the angled side wall 36 and 38 , respectively. Referring next to FIG. 14, at the corner between each of the side and front edges of the seat, the corner portions 29 , 31 of the flange 20 rests on the mounting ledges 34 or 37 , respectively.
As will be apparent to those of ordinary skill in the art, a preferred embodiment of the invention has been described above. Modifications and variations to the preferred embodiment may be made within the spirit and scope of the invention. Therefore, the invention is not to be limited to the described embodiment. To ascertain the full scope of the invention, the following claims should be referenced.
Industrial Applicability
The present invention provides a shower enclosure having a removable shower seat. | Disclosed is a removable shower seat for use in a modular shower. The seat is constructed from a plastic material and includes an elastomer coating which is molded onto the plastic substrate. The shower seat mounts to shower module wall pockets at each end, and is further supported at the rear and front corners. | 0 |
RELATED APPLICATIONS
[0001] This application claims priority to U.S. Provisional Patent Application 60/437,169, which was filed on Dec. 30, 2002 and to U.S. Provisional Patent Application 60/480,476, which was filed on Jun. 19, 2003. Both of these applications are incorporated herein by reference.
COPYRIGHT NOTICE AND PERMISSION
[0002] One or more portions of this patent document contain material subject to copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent files or records, but otherwise reserves all copyrights whatsoever. The following notice applies to this document: Copyright© 2002, Thomson Legal & Regulatory, Inc.
TECHNICAL FIELD
[0003] Various embodiments of the present invention concern information retrieval systems and knowledge-management systems, particularly such systems in a legal-research or law-firm context.
BACKGROUND
[0004] The American legal system, as well as some other legal systems around the world, rely heavily on written judicial opinions, the written pronouncements of judges, to articulate or interpret the laws governing resolution of disputes. As a consequence, judges and lawyers within our legal system are continually researching an ever expanding body of past opinions, or case law, for the ones most relevant to resolution or prevention of new disputes. Found cases are studied for relevance and are ultimately cited and discussed in documents, called work product, which, for example, advocate court action, counsel clients on likely court actions, or educate clients and lawyers on the state of the law in particular jurisdictions.
[0005] Over time, law firms, particularly large one with scores of lawyers and hundreds of clients, amass large collections of work product. In attempting to manage and leverage the value of these collections, many law firms in the last decade or so have sought to use knowledge-managements systems.
[0006] Most, if not all, of these systems have been built around document-management systems (DMSs) that assist in storing, indexing, and searching law-firm documents. The indexing and searching capability of these systems allows lawyers to reuse some of their work product, and thus have in some instances enhanced the efficiency of lawyers in developing new work product.
[0007] However, the present inventors have recognized that centering a law firm's knowledge management on document-management systems presents at least two problems. First, the document collections in these systems are generally undisciplined in the sense that they include multiple versions of the same document, non-legal documents, and so forth. Thus, searches in the DMS collections often turn up marginally relevant documents or draft documents that frustrate efforts to quickly identify the high-quality finished documents most likely to have reusable content. Second, even when apparently reusable documents are found, it is necessary for lawyers or other highly trained personnel to assess not only whether their legal arguments are of high quality, but also whether their supporting case law has been overruled, weakened, or otherwise affected by newer case law or other legal developments. (Even with online legal research services, such as the Westlaw online service, that allow one to check the validity of case law on a case-by-case basis,) this assessment is generally time consuming and thus offsets the efficiency gains of reusing work product.
[0008] Accordingly, the present inventors have identified a need for better systems, tools, and methods of managing and leveraging the accumulated knowledge within law-firm document collections.
SUMMARY
[0009] To address this and/or other needs, the present inventors have devised unique systems, methods, interfaces, and software for managing and leveraging knowledge in law firms and potentially other enterprises. For example, one system provides a single user interface for researching case law for online legal research service and identifying and accessing law-firm documents. The interface allows a user, such as an attorney, to initiate or submit a legal research query and view search results that identify not only relevant external documents from the online legal research service, but also relevant internal documents, such as briefs, client letters, and legal memoranda, from the law firm's own document collection.
[0010] Moreover, in this exemplary system, the external and internal documents are displayed with validity indicators, such as color-coded icons, that indicate whether cases they cite are still valid law, enabling the attorney to more readily assess the strength or weakness of each identified document.
[0011] Notably, the exemplary embodiment provides a seamless integration of the internal and external documents, yet the internal documents never leave the security of the law firm firewalls.
BRIEF DESCRIPTION OF DRAWINGS
[0012] FIG. 1 is a block diagram of an exemplary information system 100 corresponding to one or more embodiments of the present invention.
[0013] FIG. 2 is a flow chart corresponding to one or more exemplary methods of operating an information system and associated components that embody the present invention.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0014] The following description, which incorporates the figures and the appended claims, describes and/or illustrates one or more exemplary embodiments of one or more inventions. These embodiments, offered not to limit but only to exemplify and teach the invention(s), are shown and described in sufficient detail to enable those skilled in the art to make and use the invention(s). Thus, where appropriate to avoid obscuring the one or more inventions, the description may omit certain information known to those of skill in the relevant art.
Exemplary Information System
[0015] FIG. 1 depicts an exemplary information retrieval and knowledge management system 100 that incorporates one or more teachings of the present invention. System 100 includes a commercial online legal-data (or research) provider 110 , a law-firm information-management system 120 , and a client access device 130 .
[0016] Specifically, commercial online legal data (or research) provider 110 includes main databases 112 , reference identification database 114 , and server 116 . In the exemplary embodiment, main databases 112 contain a wide variety of legal documents, including for example, case law (judicial opinions), legislation, and journal articles. Reference identification database 114 includes a list of document identifiers and corresponding citations, with each document identifier and citation corresponding to a document within main databases 112 . Databases 112 are coupled to server 116 .
[0017] Server 116 , representative of one or more servers, includes a processing unit 1161 , and a memory 1162 . Memory 1161 , which can take the form of an electronic, magnetic, or optical computer- (or machine-) readable medium, includes one or more one or more search engines, and other modules and software, such as browser-compatible user-interface elements (UIEs) for receiving and fulfilling queries from clients.
[0018] In the exemplary embodiment, server 116 serves active or dynamic content in the form of hypertext markup language (HTML), extensible markup language (XML), or more generally a markup-language, documents or pages. To this end, the exemplary server supports the following web services or protocols: TCP/IP, SOAP (HTTP, HTML, XML), and UDDI. Additionally, the UIEs of server 116 include one or more Java scripts, applets, or other related software and data structures for serving data in association with desired interactive control or user-interface features, objects, modules, or elements. (In some embodiments, the HTML pages include URL or other embedded instructions that include one or more portions of queries submitted from an access device, such as access device 130 .) These features work in conjunction with client processor and software platforms to define one or more portions of a browser-based graphical user interface for legal research. Server 116 is coupled or couplable, for example, via an Internet Protocol (IP) network, to law-firm information-management system 120 .
[0019] Law-firm information-management system 120 includes a document-management subsystem 122 , and a knowledge-management subsystem 124 . Document-management subsystem (DMS) 122 includes a DMS database server 1221 and a DMS database 1222 . DMS database 1222 includes internal firm work-product documents, such as briefs, legal memorandum, opinions, letters, and multiple versions of same in multiple stages of completion. It may also include non-legal materials. The contents of the DMS database are generally associated with metadata profiles indicating authors, creation dates, update dates, client numbers, security settings, access restrictions and so forth.
[0020] Knowledge management subsystem (KMS) 124 includes a KMS server 1242 and a KMS database (or document repository) 1244 . KMS server 1242 , which may present one or more servers depending on loading and performance issues, includes a full-text index module, an engines-and-applications module, an HTML library module, a metadata database module, a citation index module, and a usage-and-tracking module, all of which are not shown as separate items in FIG. 1 .
[0021] In the exemplary embodiment, full-text-indexer module is used to facilitate general retrieval of documents from KMS database by indexing documents and/or providing index data. Engines-and-applications module includes the following engines and applications: citation-identification engine, full-text search engine, KeyCite Flags engine (see appendix for further details); scheduler application for handling migrating documents from DMS database, DMS integration components, and system administration tools.
[0022] HTML library module stores HTML version of each document contained in the research repository, including KeyCite flags and tags. Metadata database module 1242 D stores descriptive information and attributes of documents contained in the KMS database, includes information from the DMS database. Citation index module indexes the citations relationships between documents to maintain flags and tags on citations. And, usage-tracking database stores and maintains a historical log of all search and retrieval activity containing detail information by document name, author, area of law, and user ID.
[0023] KMS database stores a selected set of high-quality internal work-product documents. In the exemplary embodiment, these documents are copies of documents selected from DMS database 1222 . When copied into KMS database 1244 , one or more portion of the metadata profile data is also incorporated into KMS database.
[0024] Law-firm information-management system 120 and online legal-research provider 110 are both communicatively coupled or couplable, via a local-area network (such a corporate intranet) or wide-area network (such as the Internet) to access device 130 .
[0025] Access device 130 , which is generally representative of one or more access devices within a business organization, such as a law firm, takes the exemplary form of a workstation. In addition to a keyboard 131 (lower left hand corner), a mouse (graphical pointer) 132 , and a display 133 , access device 130 includes a processing unit 134 , a memory module 135 , and a browser-compatible legal-research interface 136 .
[0026] More particularly, processing unit 134 includes at least one processing circuit. Memory module 135 , which takes the form of one or more electronic, magnetic, optical machine-readable mediums, includes operating system 1351 , a browser application 1352 , and a word processor application 1353 .
[0027] Operating system 1351 , which cooperates with processing unit 134 and takes the exemplary form of the Microsoft Windows operating system, includes a set of user-interface objects, modules, or elements, accessible via application programs such as browser application 1352 . Browser application 1352 takes exemplary form of a Microsoft Internet Explorer™ or Netscape Navigator browser, cooperates with operating system 1321 and externally provided data, coded instructions (collectively UIEs) from servers such as (external legal-research) server 116 and internal KMS server 1242 , to define and render, on display 133 , browser-compatible legal-research interface 136 .
[0028] Legal-research interface 136 includes a query portion 1361 , an external re-results portion 1362 , an external document display portion 1363 , an internal-results portion 1364 , and an internal document display portion 1365 . In the exemplary embodiment, portions 1361 - 1365 are not necessarily displayed or accessed simultaneously. For example, the interface can include tabs and full-screen-display options that enable the user to focus the display on particular portion of the data or interface portions. One embodiment provides one folder tab to invoke display of a combined listing of internal and external results with corresponding indicators to distinguish internal results from external ones and the other to invoke display of internal results only.
[0029] Query portion 1361 includes a label portion L and one or more associated interactive user-interface (UI) elements (objects, features, or widgets), E and EE (referred to hereinafter as label portion 1361 L, and elements 1361 E and 1361 EE.) Label portion 1361 L is defined to display a query-indicator label, such as “Search Based on this New Citation,” “KeyCite this Citation, or “Search these Databases,” to indicate to a user that some form of query input is expected within this portion of the interface. UI element 1361 E accepts input from a user. In the exemplary embodiment, this UI element takes the form of a text box or menu, with the menu enabling the use to select a target for the query, such as the KMS database. As a default, the exemplary embodiment will run the query against the KMS database in combination with any other database set that is selected. (Some embodiments provide a set of UI elements that enable the user to select from a number of predefined category- or subject-matter-specific queries. The queries are defined, for example, by expert legal researches in the specific legal areas. A hierarchical organization or outline of the queries facilitates user selection of the appropriate query by the user. The user may also view the details of the predefined queries and modify as desired prior to submission.)
[0030] UI element 1361 EE allows a user to initiate submission and execution of a query defined via user-interface element 1361 E. The exemplary embodiment provides this feature in the form of a “go” button, which upon actuation results in transmission of the defined query (or relevant portion of it) to not only main database 112 (server 116 ), but also to KMS database XYX for fulfillment. (In some embodiments, the query is submitted only to KMS database XYX.)
[0031] External-results portion 1362 is defined to display search results obtained or received from online legal-research provider 110 , or more precisely its main database 112 . In the exemplary embodiment, external-results portion 1362 includes one or more document identifiers or descriptors 1362 D which are displayable in association with corresponding user-interface element L 1 . Descriptor 1362 D provides information regarding a corresponding external-results document within database 112 . In the exemplary embodiment, this information includes a title T 1 , metadata M 1 , and a case validity flag F 1 . UI element L 1 , for example a hyperlink, provides an option which can be invoked for example, by clicking, to retrieve and display the document(s) associated with descriptor 1362 D, as indicated by document display 1363 .
[0032] Document display 1363 , which in some embodiments is presented in a spit-screen along a listing of the internal and/or external results, displays at least a portion of the external document associated with UI element L 1 . The document includes text (denoted by the broken lines) and legal citations CA and CB, which are respectively associated with case-validity flags FA and FB and hyperlinks LA and LB. Selection of hyperlinks LA and LB all a user retrieve the documents corresponding to the citations from online legal-research provider 110 .
[0033] Internal-results portion 1364 is defined to display results of querying internal firm database, KMS database 1244 . In the exemplary embodiment, internal-results portion 1364 includes one or more sets of document-specific UI elements, such as UI element set 1364 D, one or more of which are displayable in association with a corresponding UI element L 2 . Each UI-element provides data or access to data about the contents of an associated internal-results documents, such as a document title T 2 , metadata M 2 , case-law validity flag F 2 , and law-firm rating R 2 .
[0034] More precisely, metadata M 2 includes one or more portion of the metadata associated with the original DMS copy of the identified document. (The exemplary embodiment populates KMS database with copies of documents selected from DMS database.) In the exemplary embodiment, this includes author, client, document ID, dates of creation and revision, etc. Case-law validity flag F 2 provides an indication of the validity of case law cited within the corresponding firm document. Law-firm rating R 1 provides an indication of the utility and/or quality of the document as determined by previous law-firm users of the document.
[0035] UI element L 2 , similar to UI element L 1 , provides a user option to retrieve and display the internal document(s) associated with descriptor 1364 D. Exercising this option results in a display document display 1365 .
[0036] Document display 1365 , which in some embodiments is presented in a spit-screen along a listing of the internal and/or external results, displays at least a portion of the internal document associated with UI element L 2 . The document includes text (denoted by the broken lines) and legal citations CA and CX, which are respectively associated with case-validity flags FA and FB and hyperlinks LA and LX. In addition to providing a visual indication of case-law validity, the case-validity flags can be selected in some embodiments to cause retrieval and/or display of further information regarding the nature of the flags. Hyperlinks LA and LX all a user retrieve the documents corresponding to the citations from online legal-research provider 110 . In addition to the text and citations, document display 1365 provides a firm-name label FN to clearly identify the document as an internal law firm document, a title label T 2 for indicating the title of the corresponding internal document, and a load-copy UI element LC for enabling user to initiate loading of a copy of the corresponding internal document directly into a word processor application of access device 130 for use in generating a new work product document. Moreover, document display portion 1365 also includes a ratings UI-element R 1 which enables a user to see the current law-firm-user rating of the document as well as to rate the current document. Figure X shows an exemplary set of UI elements for achieving this rating.
Exemplary Method of Operation
[0037] FIG. 2 shows a flow chart 200 of one or more exemplary methods of operating an information-management system, such as system 100 . Flow chart 200 includes blocks 210 - 280 , which are arranged and described in a serial execution sequence in the exemplary embodiment. However, other embodiments execute two or more blocks in parallel using multiple processors or processor-like devices or a single processor organized as two or more virtual machines or sub processors. Other embodiments also alter the process sequence or provide different functional partitions to achieve analogous results. Moreover, still other embodiments implement the blocks as two or more interconnected hardware modules with related control and data signals communicated between and through the modules. Thus, the exemplary process flow applies to software, hardware, and firmware implementations.
[0038] At block 210 , the exemplary method begins with a law-firm user, such as an attorney or paralegal, initiating a search session with online legal-research system 110 . In the exemplary embodiment, this entails the user at access device 130 logging onto a law-firm network using security measures, such as an assigned username and password. After login, the user then launches and directs the Internet browser within access device 130 to connect to the online legal research system. In some embodiments, the user enters a separate username and password to initiate the search session, and in others the previous network login suffices. Execution continues at block 220 .
[0039] Block 220 entails displaying or otherwise loading and presenting one or more portions of legal-research user interface 156 . In the exemplary embodiment, this entails server 116 of online legal-research system 110 sending an HTML document (or webpage) that includes scripts, applets, and associated data for causing access device 130 to display query portion 1361 of user interface 136 . For users at law firms that have a knowledge management system, such as management system 100 , which is provided or authorized by the online legal research system, the associated data includes at least one firm-name label to use in labeling specific portion of the user interface as well as the name of KMS server 1242 , which is configured and/or authorized to access KMS database 1244 . Execution continues at block 230 .
[0040] Block 230 entails the user defining and submitting a query. In the exemplary embodiment, this entails the user defining a query using query portion 1361 of interface 136 . Query portion includes features, such as a text box or pull-down menus that enable the user to define a citation, natural-language, or terms-and-connectors query. The interface also presents the user an option to specify the scope of the search or query as including one or more databases within online legal research system and/or at least one internal law firm database. Options related to identifying the internal law firm databases are labeled based on the firm-name label provided by the online legal research system. After defining the query, the user submits it to system by actuating a UI element, such as a “go” button, using an input device, such as a mouse or keyboard. The query is then communicated over the Internet to server 116 and KMS server 1242 .
[0041] Block 240 entails searching databases at one or both of the online legal search system and the law-firm information management system based on the submitted query. In the exemplary embodiment, online legal-search system 110 , or more precisely, server 116 executes or causes execution of the query against the requested databases, and returns results the search (external results) to access device 130 in the form of HTML documents with associated control features and data. If the query was defined to include law-firm databases, an applet, script or other device is returned along with the external results of access device 130 to trigger or cause access device to call KMS server 1242 to execute the query against an internal law-firm database, such as KMS database 1244 . Some embodiments may call the KMS server concurrently with submission of a query identifying an internal law-firm database. In any case, KMS server executes the search against the KMS databases and serves results in the form of a mark-up language document, such as HTML, to access device 130 . Execution of the exemplary method continues at block 250 .
[0042] Block 250 entails presenting the search results. In the exemplary embodiment, this presentation entails presenting the internal results and the external results via the browser interface in association with one or more sets of UI elements (or interactive control features), as shown in FIG. 1 .
[0043] Block 260 entails displaying an internal law-firm document from internal results set. In the exemplary embodiment, this entails the user selecting a UI element, such a link, associated with one of the listed internal documents and the KMS server retrieving the document from the KMS database and serving it to the access device. Notably, the KMS server automatically updates the document to the current state of the law—that is, current validity flags are inserted next to all of the authorities in the document. The KMS server requests these from the online legal-research provider—in real time—an inserts them prior to serving up the pages to the access device. Another feature of this interface allows the use to click on an UI element and move the mouse cursor to each place in the document that contained terms from the search, for example, a citation in the case of a citation search.
[0044] Block 270 entails loading the displayed internal document into a word-processing application program. In the exemplary embodiment, this entails the user selecting a “load copy” icon LC on the internal-document display portion 1365 of interface 136 . In response, user interface 136 , which includes an appropriate application program interface, launches or otherwise communicates with the word-processing application to load the document from interface 136 into the word-processing application for user modification. In response, tracking system data within KMS server 1242 is also updated to reflect usage of this internal document. (The exemplary system generally tracks everytime a user clicks on something, specifically creating a usage record indicating the date, time, user, client-mater, type of transaction.)
[0045] Block 280 saves the modified copy of the internal document in the DMS database as a new work product document. In the exemplary embodiment, this entails the user also providing metadata profile data for the new document.
Exemplary Method of Building the Research Repository
[0046] In the exemplary system of FIG. 1 , knowledge-management subsystem 120 includes KMS database 1244 , which serves as a research repository of documents selected from DMS database 1224 . KMS server 1242 includes software (that is, coded instructions) for automatically migrating or mirroring select documents from firm's DMS or network file system to the KMS database 1242 .
[0047] In the exemplary embodiment, this migration process initially entails retrieving one or more documents from DMS database, for example, using administrator defined queries and executing those queries on a scheduled basis or event-driven basis. Next, the exemplary method entails converting the retrieved documents into a markup language, such as HTML, subsequently indexing the converted documents based on citations and text. The next series of operations include storing citation relationships, storing the HTML documents with tagged citations, and storing document profile data all in a relevant portion of the KMS server.
Appendix
[0048] The following appendix includes a detailed user guide and an administrative guide of an exemplary knowledge management-system and related software and components that corresponding to one or more embodiments of the present invention.
Conclusion
[0049] The embodiments described above are intended only to illustrate and teach one or more ways of making and using the present invention, not to restrict its breadth or scope. The actual scope of the invention, which embraces all ways of practicing or implementing the teachings of the invention, is defined only by one or more issued patent claims and their equivalents. | The present inventors devised unique systems, methods, interfaces, and software for managing and leveraging knowledge in law firms and potentially other enterprises. For example, one system provides a single user interface for researching case law for online legal research service and identifying and accessing law-firm documents. | 6 |
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to coated water-vapor-pervious and fungus-resistant wovens, especially industrial wovens, to a process for producing same and, to their use for the production of sun protection and weather protection articles such as tent materials, boat covers and the like.
2. Related Technology
Water-vapor-pervious textile fabrics are known in particular from the use sectors of functional sports and protective clothing and also various medical sectors. Common processes for producing water-vapor-pervious textiles from the sectors cited above are known in particular under the designations of “Goretex” and “Sympatex,” which work according to the principle of producing microporous structures.
Watertight yet moisture-pervious coated textile fabrics and processes for their production are inter alia described in DE 2948892 C2. The processes described therein utilize a polyurethane solution in an organic solvent, producing the microporous layer of polyurethane by coagulation.
Further processes for producing polyurethane-coated textile fabrics which are breathable and water repellent are described for example in DE 3633874 C2. The process described in this patent specification utilizes two aqueous polyurethane dispersions which are applied in succession wet on wet.
However, it has been determined that the water vapor transmission rate is not always satisfactory. In addition, condensates form very frequently in the pores of the coatings. One of the disadvantages of this is that fungi form in these condensates. Inevitably, fungi will also spread in those spaces which are actually to be protected by the coated wovens. Unsightly matt deposits form on the fittings of the interior spaces of ships such as yachts and the like and confer an unsightly appearance on objects in the interior.
It is another frequent occurrence, when thus coated textiles are used as a covering on ships and the coverings develop dents or dips in which water can collect, that the water pressure on the coated textile will increase over time to such an extent that water in liquid form as well as in vapor form is able to pass through the coated woven and get into interior to be protected.
Although there already are a whole series of water-vapor-pervious polyurethane-coated wovens, there is still a need for improved polyurethane-coated wovens and for simple processes for their production and in particular for coated wovens which are particularly useful for producing sun protection and weather protection articles.
SUMMARY OF THE INVENTION
The invention provides a process for producing such coated fabrics, which possess good water vapor perviousness and good water pressure resistance, and in addition possess improved fungus protection properties, are oil, soil, and water-repellent, and which in addition are also weathering-resistant.
Accordingly, the invention provides a process for producing coated water-vapor-pervious and fungus-resistant wovens, wherein a washed woven is impregnated with an aqueous impregnant containing a fungicide and a hydrophobicizer, dried, then coated with an aqueous dispersion of a polyurethane likewise containing a fungicide without further additives such as new color-conferring additives, dried and subsequently reimpregnated with an aqueous hydrophobicizer and dried.
DETAILED DESCRIPTION
The aqueous impregnant preferably comprises 1%-5% and especially 2%-4% by weight of fungicide. The aqueous impregnant advantageously contains 0.2% to 2% and preferably 0.4% to 1% by weight of a hydrophobicizer.
The aqueous dispersion preferably contains hydrophilic polyurethanes.
It is further advantageous when the impregnated and dried woven is at least once coated with an aqueous polyurethane dispersion.
It is further advantageous when the impregnating is effected by pad-mangling or spraying.
The invention further provides coated water-vapor-pervious and fungus-resistant wovens producible by one of the processes indicated above.
The wovens of the invention preferably have a water vapor transmission rate of 800 to 2800 g/m 2 ×24 h at 20-50° C.
Of particular advantage are coated, water-vapor-pervious and fungus-resistant wovens having a water pressure resistance of 800 to 1800 mm hydrohead.
The process of the invention can be carried out as follows.
The initial step is to produce a woven fabric in a conventional manner. The wovens are in particular industrial wovens, which have a higher basis weight and tensile strength than wovens for purely textile purposes. The basis weight of the wovens is advantageously in the range from 150 to 450 g/m 2 .
The woven is then cleaned, for example by washing it in the loom state by means of a jigger or continuous washing process, to remove in particular residual spin finish and the like.
The woven thus washed and dried is then impregnated with an aqueous impregnant. This impregnant comprises one or more fungicides and also one or more hydrophobicizers. The woven is then impregnated so thoroughly that the fibers and yarns are fully enveloped by impregnant. This is necessary to obtain uniform coating in the subsequent coating process.
After the impregnating step, the woven thus impregnated is dried. The fungicide is generally present in the impregnant in an amount of 20-40 g preferably 30 g per liter of water. The impregnant further comprises a hydrophobicizer in an amount of for example 4-10 g especially 7 g per liter of water.
After the impregnating step, the woven thus impregnated and dried is coated. Aqueous dispersions of hydrophilic polyurethanes are used for coating. The aqueous dispersion shall comprise sufficient polyurethane to ensure that an adequate amount of polyurethane is applied to the woven. The amount is advantageously determined such that the fabric comprises between 30 and 50 g of coating add-on per square meter of area, these indications of amount relating to polyurethane solids.
The aqueous coating further contains a fungicide, preferably the same fungicide, or else if appropriate a fungicide which is similar or of the same type, as used in the impregnation. The coating may further contain customary additives, such as color pigments for example.
Once a sufficient and uniform coating has been applied to the woven, the woven is dried and is then subjected to a further impregnation with an aqueous system containing a hydrophobicizer, preferably 3 to 5 g per 100 g of aqueous composition. This reimpregnation provides an improvement in oil, water and soil repellency.
Wovens thus coated possess in particular good water vapor perviousness, a high water pressure resistance, good oil, soil and water repellency and also excellent fungus resistance. These performance characteristics last throughout the entire use life, so that the protected interior likewise remains protected against moisture and fungal colonization.
The wovens thus coated are very useful according to the invention for solar protection and weather protection articles. To be identified in particular here are tent materials, tent roofs, beer tent fabrics, boat covers, boat winter storage covering, boat summer covering, sprayhoods in the boat sector, bow protection panes on boats, including in particular those sheetlike structures which are intended to protect on-boat rooms and spaces, for example cabins, against moisture and fungus formation.
The yarns for the wovens may utilize polyester, in particular polyethylene terephthalate filaments and fibers, for example filament yarns, continuous filament fibers or staple fiber yarns, fibers composed of acrylics, cotton and also blends of synthetic sand natural fibers or manufactured fibers such as cellulosic fibers.
Useful further ingredients to be added at impregnation or coating include customary additives, for example color pigments.
The example which follows illustrates the invention:
Example
The base fabric to be finished in this operative example is a woven acrylic fiber fabric having a basis weight of about 300 g/m 2 , this fabric having been produced from spun-dyed staple fiber yarns.
The substrate is washed in a first step of the process by means of a jigger or continuous washing process to remove residual substances such as spin finishes from the loom state fabric.
The next step consists in a preimpregnating operation which insures, on the one hand, that the coating film can be uniformly applied in the subsequent coating process and, on the other, the fungicide is uniformly distributed in the fabric.
In this preimpregnating operation, the fungicide is present in an amount of 20 to 40 g-preferably 30 g-per liter of water and a hydrophobicizer is present in an amount of 4 to 10 g—for example 7 g—per liter of water.
The effect of the hydrophobicizer is that the coating is applied as a film on the surface of the fabric in the next step.
The subsequent coating process provides for uniform application of a water-vapor-pervious polyurethane—namely a hydrophilic aliphatic polyurethane—(or else a mixture of this polyurethane with another polyurethane) in the form of an aqueous dispersion in a one-pass process, the amount applied to the fabric being between 30 and 50 g/m 2 -preferably 40 g/m 2 .
This amount is to be understood as meaning that amount of solids which is present in dissolved form in an aqueous solution of 100 g total weight which is used per m 2 of fabric to be coated.
The coating, i.e. the aqueous dispersion, further comprises the fungicide of the same type in a concentration of 3% to 5%-4% for this example—i.e. 4 g in 100 g of aqueous dispersion.
Finally, the fabric thus coated is subjected to a reimpregnation through a customary pad-mangling process in which the hydrophobicizer is again present in an amount of 4 g of 100 g of aqueous solution, whereby adequate oil, water and soil repellency is additionally achieved on the textile end product. | Coated, water-vapor-pervious and fungus resistant wovens, their production and also their use as sun and weather protection articles, a precleaned industrial woven fabric being treated at least once with an aqueous impregnant comprising a fungicide and a hydrophobicizer. The fabric thus impregnated and then dried is subsequently coated with an aqueous polyurethane dispersion which likewise contains a fungicide. After drying, the coated fabric is reimpregnated. The wovens are notable for fungus resistance, good water vapor perviousness and good watertightness against a high hydrohead in particular. | 3 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] Not Applicable
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
REFERENCE TO A COMPUTER PROGRAM APPENDIX
[0003] Not Applicable
BACKGROUND OF THE INVENTION
[0004] 1. Field of the Invention
[0005] The present invention pertains to content selection mechanisms within digital content-laden material, and more particularly to embedding MPEG-7 content descriptions as META data within the header of a document containing markup language to increase specificity of content selection.
[0006] 2. Description of the Background Art
[0007] The proliferation of digital material, such as over the Internet, has provided persons utilizing such content with nearly an unlimited amount of text and multimedia from which to choose. Attached, however, to the advantages of this content proliferation are the practical difficulties associated with searching, or otherwise selecting, digital content elements to best meet the content needs of the searcher. The large amount of digital material, such as various forms of multimedia content, that can be returned from a content search often require inordinate amounts of human interaction to select the most appropriate items in relation to the desired content. Large content repositories, such as those providing stock photographs over the Internet, have utilized diverse methods of cataloging their content to speed the selection process.
[0008] The Moving Pictures Expert Group, known as the MPEG working group of ISO/IEC, has proposed a standard referred to as MPEG-7 for describing content, with particular emphasis on multimedia content such as video, images, music, speech, audio, and so forth. It should be appreciated that MPEG-7 provides a standard for representing information about the content, and does not provide a mechanism for representing actual content, as were found in the previous standards, such as MPEG-1 and MPEG-2.
[0009] Included within the content descriptions within MPEG-7 are the use of descriptors that can be utilized to describe the various features of the multimedia content, and the use of description schemes which provide predefined structures of descriptors and their relationships. The standard provides for differing levels of granularity and user-group specificity within content descriptions. For example, the description of an image content element may describe the shape, size, and color, while a higher level of abstraction may for instance describe mood, genre, semantics and relationships which exist within associated content. Machine generated information, such as color histograms and audio characterization data may also be included within the MPEG-7 descriptions. Each description may also contain content type descriptions including: form, such as data size and coding scheme; classification, such as parental ratings and usage area; access conditions, such as copyright information, price, and contact information; context, such as from where the content was collected or created; links to other relevant content, and so forth. It will be appreciated that various levels of content information may be contained by the MPEG-7 standard for indexing or cataloging multimedia content. However, users or agents searching for select content do not have a convenient method for utilizing MPEG-7 content descriptions to facilitate their searches.
[0010] Therefore, a need exists for a method and system of incorporating MPEG-7 content descriptions into accessible content, such as content available over the Internet, to facilitate rapid and accurate content selection. The present invention satisfies those needs, as well as others, and overcomes the deficiencies of previously developed systems.
BRIEF SUMMARY OF THE INVENTION
[0011] The present invention is capable of providing searchable MPEG-7 content descriptions in association with digital material, particularly those containing multimedia content. The system and method can be implemented within a variety of infrastructures, such as within network enabled computers communicating over the World Wide Web. Generally, the invention provides for the insertion of one or more content descriptions according to the MPEG-7 multimedia content description standard into an element of digital material to allow parameterized content-related searches.
[0012] The MPEG-7 content description is received, generated, or a combination thereof within a content description definition routine executing on a computer system. The content description may be received through an interface routine into the content description definition routine, generated by a characterization routine which determines the characteristics of content elements to be represented as MPEG-7 content, generated by a conversion routine adapted for converting content information from a format that is not compliant with MPEG-7 into a compliant MPEG-7 format, generated from user input collected within a human interface capable of collecting objective and subjective characterization data about the content in response to human interaction, and combinations thereof. The content description, therefore, may be created from information received about the digital material object, determined by translations of content information, determined by direct characterization, determined with human intervention, and so forth along with combinations thereof. By way of example, information may be received in formats other than MPEG-7 and translated into standard descriptor formats, or less preferably included into non-normative parts of a descriptor. Content may be characterized, such as by utilizing algorithms to create a histogram of colors which are found in a content element, whereupon the characterization information is subsequently formatted into an MPEG-7 content description. It will be appreciated that the digital material object may contain numerous individual content elements, for example as may be found within an HTML web page containing text, graphics, and audio elements. The generation of the content description may therefore include the characterization, or alternatively the receipt, of content information relating to the elements of content and preferably their respective interrelation, if applicable. The MPEG-7 description is then embedded within the digital material to thereby augment the content with the additional descriptive information provided under MPEG-7. The description is generally provided by way of descriptors and description schemes that are embedded within a META tag inserted into the header of the digital material object. The structure of the inserted content description containing, by way of example, a META tag, opening delimiter, one or more levels of content descriptions, and a closing delimiter.
[0013] An object of the invention is to provide a mechanism for embedding content descriptions within digital material objects having headers, such as those containing multimedia elements.
[0014] Another object of the invention is to provide a mechanism for embedding information that describes layers of content elements.
[0015] Another object of the invention is to provide a method of embedding content information that conforms to an accepted standard so that content from various providers, including geographically disbursed providers, may be equally considered during a search.
[0016] Another object of the invention is to provide a simple method of embedding content which is applicable to various documents written in a markup language that contain a header, such as SGML and subsets which include HTML, XML, and WAP.
[0017] Further objects and advantages of the invention will be brought out in the following portions of the specification, wherein the detailed description is for the purpose of fully disclosing preferred embodiments of the invention without placing limitations thereon.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] The invention will be more fully understood by reference to the following drawings which are for illustrative purposes only:
[0019] [0019]FIG. 1 is a schematic of a system for embedding MPEG-7 content descriptions within a digital material object according to the present invention, shown for use with content and information repositories comprising either local databases or network derived resources.
[0020] [0020]FIG. 2 is a flowchart of a process for embedding the content descriptions within a digital material object according to an embodiment of the present invention.
[0021] [0021]FIG. 3 is a listing of an HTML header segment which exemplifies META tag use according an aspect of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0022] Referring more specifically to the drawings, for illustrative purposes the present invention is embodied in the systems and methods generally shown in FIG. 1 through FIG. 3. It will be appreciated that the systems may vary as to configuration and as to details of the elements, and that the methods may vary as to the specific steps and sequence, without departing from the basic concepts as disclosed herein.
[0023] [0023]FIG. 1 illustrates a system 10 according to the invention for embedding MPEG-7 content descriptions within the headers of digital material objects so that subsequent searches on the augmented content may be performed with more speed and accuracy. Content may be retrieved from a variety of source repositories 12 , which include local and remote databases 14 , along with network based resources 16 such as servers connected to the Internet. Information which characterizes the content may be provided by the same source repository 12 , retrieved from a third party, or performed by a characterization routine 18 . A digital material object 20 is shown comprising content 22 and a header 24 that may follow any of various markup language formats including SGML and subsets that include HTML, XML, WAP, and others. Digital material object may be characterized within routine 18 that performs summarizing 26 of the content, for example the color based histograms, size, type, and other information as may be extracted from the content. Additional characterization data may be optionally derived from human intervention 28 , wherein an operator can enter characterization data based on more subjective criteria about the content object, such as genre, theme, and classification. The characterization information is preferably generated directly into an MPEG-7 description for use by an embeddable description building routine 30 which creates an insertable META tag description 32 which is then inserted by an insertion routine 34 within the digital material object 20 to create a new digital material object 36 augmented with MPEG-7 content descriptions within the enlarged header 38 , while maintaining identical content 22 . It will be appreciated that information about digital material object 20 may be fully or partially obtained from a database 14 or via a network 16 for use within the system and may be obtained in a variety of formats. The information may additionally, or alternatively, be received in an MPEG-7 format 40 whereupon it may be utilized separately, or in combination with other information for use by the embeddable description building routine 30 into a resultant MPEG-7 content description 32 that is afterward inserted by insertion routine 34 into the digital material object 36 . Content information may be additionally, or alternatively, received in various other formats requiring manipulation by a conversion routine 42 . The provided information 44 , which is not compliant with MPEG-7, passes through a converter routine 46 which interprets the content, often utilizing mapping information which associates the format of the received content to MPEG-7 format, whereupon a conversion is performed and the resultant MPEG-7 information is used singly, or in combination with, other information by the embeddable description building routine 30 to create the MPEG-7 content description 32 which is inserted by insertion routine 34 into header 38 of digital material object 36 . The resultant digital material object, augmented with content information, is ready to be utilized within searches and is shown being deposited back to a repository 12 that may comprise remote or local databases 14 and internet resources 16 . Although, the augmented content is shown being returned to the same repository 12 , the augmented content may alternatively be deposited to other repositories or through various communication media.
[0024] It is anticipated that content providers, utilizing the system to augment existing content with MPEG-7 content descriptions, would typically perform off-line conversion processes on the database in-toto, thereby reducing issues relating to mixed versions and maintenance. The entire content repository would thereby be converted to add the new content information prior to the database being brought up, or restored, to active on-line status. It will be appreciated, however, that the system may be alternatively utilized by various entities for a number of applications which facilitate content searches and management.
[0025] [0025]FIG. 2 illustrates the general process of embedding the MPEG-7 content information within a digital material object. The process starts at block 50 and information is obtained at block 52 about the content laden object. The aforementioned methods of receiving, converting, and characterizing may be utilized in combination or separately to build content information to the desired degree of comprehensiveness. It will be appreciated that information from a number of sources can be agglomerated in the building of content information. Any information which was received but is not MPEG-7 compliant is converted at block 54 to MPEG-7 format. The content object is then modified starting at block 56 with the insertion of opening delimiters including META tag name, after which the MPEG-7 content description is inserted at block 58 , followed by embedding of the closing delimiter 60 . It will be appreciated that the description preferably comprises a series of layers commensurate with the object or objects being described within the MPEG-7 content description. The new augmented object is then stored as per block 62 as a target for subsequent enhanced searching, whereupon the process is completed at block 64 .
[0026] [0026]FIG. 3 is a listing of a portion of an HTML header containing META tags and exemplifying the insertion point of the MPEG-7 content descriptions within the header information of the digital material object. It will be appreciated that the META names may be altered, and the structure modified without departing from the present invention. A “META NAME” for the embedded content description was selected as “MPEG7Unit” which is followed by the MPEG-7 content description. Portions of additional header elements are exemplified by the META tag “Robot”, while the termination of the header is shown by the transition from a “</HEAD>” to a “<BODY>” which contains the web page. It will be appreciated that the MPEG-7 content descriptions may be inserted as a META tag within various document formats which contain headers. By way of example these formats include machine-to-man browser entities, such as the aforementioned web page, and machine-to-machine transaction sessions that are established through the use of a headered entity. In either exemplified case, the META tag MPEG-7 content information may be utilized directly or through programmatic means to increase the speed and accuracy of searching content contained therein.
[0027] Accordingly, it will be seen that this invention provides a method and system for augmenting documents and other content containing digital material objects with content descriptions that can be utilized for increasing the speed and accuracy of content related searches. It will be appreciated that the method and system may be implemented using a variety of computer systems, and that the method is applicable to various forms of content-laden digital material objects containing headers. Specific instances of embedded MPEG-7 content descriptions have been described by way of example, and it should be realized that the specific syntax and use of delimiters can be widely varied without departing from the present invention.
[0028] Although the description above contains many specificities, these should not be construed as limiting the scope of the invention but as merely providing illustrations of some of the presently preferred embodiments of this invention. Therefore, it will be appreciated that the scope of the present invention fully encompasses other embodiments which may become obvious to those skilled in the art, and that the scope of the present invention is accordingly to be limited by nothing other than the appended claims, in which reference to an element in the singular is not intended to mean “one and only one” unless explicitly so stated, but rather “one or more.” All structural, chemical, and functional equivalents to the elements of the above-described preferred embodiment that are known to those of ordinary skill in the art are expressly incorporated herein by reference and are intended to be encompassed by the present claims. Moreover, it is not necessary for a device or method to address each and every problem sought to be solved by the present invention, for it to be encompassed by the present claims. Furthermore, no element, component, or method step in the present disclosure is intended to be dedicated to the public regardless of whether the element, component, or method step is explicitly recited in the claims. No claim element herein is to be construed under the provisions of 35 U.S.C. 112, sixth paragraph, unless the element is expressly recited using the phrase “means for.” | A system and method for augmenting digital material with MPEG-7 content descriptions to enhance searching and selection of the digital material. Pursuant to the collection of content information about the digital material, either through receipt or content characterization, a set of MPEG-7 descriptor schemes and descriptors are created for constituent elements of the content. The MPEG-7 descriptions are structured as META tags, including predetermined opening and closing delimiters, which are inserted within the header field of the digital material. The MPEG-7 content description data may contain multiple content levels describing levels of associated embedded content. By way of example, use of MPEG-7 content descriptions within a web site (or internet transaction session) can improve the speed and accuracy of content selection. | 6 |
TECHNICAL FIELD
[0001] The present invention relates to a compound as defined by the formula (I) or formula (I′) or a pharmaceutically acceptable salt thereof for use in preventing or treating an ocular disease in animal including human. This invention relates to use of the said compound or a pharmaceutically acceptable salt thereof for the manufacture of a medicament for preventing or treating an ocular disease. The invention relates to a method for preventing or treating said diseases comprising administering the said compound or a pharmaceutical composition comprising the same to animal including human. Further, this invention relates to a pharmaceutical composition or a kit comprising the said compound or a pharmaceutically acceptable salt thereof for preventing or treating said diseases.
BACKGROUND ART
[0002] Prostaglandins play a major role in the inflammation process and the inhibition of prostaglandin production, especially production of PGG 2 , PGH 2 and PGE 2 , has been a common target of antiinflammatory drug discovery. However, common non-steroidal antiinflammatory drugs (NSAIDs) that are active in reducing the prostaglandin-induced pain and swelling associated with the inflammation process are also active in affecting other prostaglandin-regulated processes not associated with the inflammation process. Thus, use of high doses of most common NSAIDs can produce severe side effects, including life threatening ulcers, which limit their therapeutic potential. An alternative to NSAIDs is the use of corticosteroids, which have even more drastic side effects, especially when long term therapy is involved.
[0003] NSAIDs prevent the production of prostaglandins by inhibiting enzymes in the human arachidonic acid/prostaglandin pathway. The expression of cyclooxygenase-2 (COX-2) is specifically induced in the pathological conditions such as inflammation, pain, and cancer, and is involved in the generation and maintenance of these conditions. According to the line, a series of drugs called coxibs such as celecoxib, rofecoxib, valdecoxib, parecoxib, and etoricoxib have been developed.
[0004] Coxib-drugs are useful for the treatment of diseases mediated by cyclooxygenase-2, such as inflammation, pain, cancer, fever, osteoarthritis, rheumatoid arthritis, migraine, neurodegenerative diseases, cardiovascular disease, osteoporosis, asthma, lupus and psoriasis, dysmenorrhea, premature labor, gout, ankylosing spondylitis, bursitis, heat burn, sprain, and contusion (non-patent literature 1).
[0005] The benzopyran, naphtopyran, dihydroquinoline, benzothiopyran and dihydronapthalene derivatives, represented by the formula (I) or formula (I′) in this invention are disclosed in the patent literature 1, and preferably selectively inhibit cyclooxygenase-2 over cyclooxygenase-1. Among them, the benzopyran derivative, for example, affords more potent analgesia and more rapid onset of effect than ibuprofen which is the first choice among the conventional drugs. Furthermore it has been confirmed in the preclinical studies that the benzopyran derivatives have lower renal problems which are a matter of concern in conventional COX-2 inhibitors and NSAIDs.
CITATION LIST
Patent Literature
[0000]
{PL 1} JP Patent No. 4577534
Non-Patent Literature
[0000]
{NPL 1} Inflamm Res. 2000 August; 49(8):367-92
SUMMARY OF INVENTION
Problems to be Resolved by the Invention
[0008] In general, active ingredients involved in coxib-drugs have a sulfonamide group, whereas a compound of formula (I) or a compound of formula (I′) is a unique chemical structure, which has neither sulfonamide group nor alkylsulfonyl group but has a carboxylic acid group which may be esterified. Hereafter in the present specification, such coxib-drugs or coxib-compounds, which have neither a sulfonamide group nor an alkylsulfonyl group but have a carboxylic acid group, are called the third generation coxib-drugs or third the generation coxib-compounds. Therefore, the third generation coxib-drugs have a unique pharmacological effects which are never seen in conventional COX-2 inhibitors. In the present invention, a compound represented by a compound of formula (I) may be the same as that of formula (I′).
Means of Solving the Problems
[0009] When applying the third generation COX-2 inhibitor of the formula (I) or formula (I′) to some ocular disease models, the present inventors have surprisingly found that the said inhibitor has an excellent effect against chorioretinal neovascularization. The inventors establish a technical idea that a compound of the present invention is useful for ocular diseases, and have completed the present invention by further examinations.
[0010] Namely the present invention discloses:
[0000] [1] A compound as defined by the following formula (I′) for use in preventing or treating an ocular disease in animal including human, which is referred to as “a compound of the present invention”;
[0000]
[0000] wherein
X is selected from O, S and NR a ;
R a is selected from hydrido; C 1 -C 3 -alkyl; (optionally substituted phenyl)-methyl; and phenylmethyl; wherein the phenyl ring is substituted by 1 to 3 substituents independently selected from C 1 -C 6 -alkyl, hydroxyl, halo, C 1 -C 6 -haloalkyl, nitro, cyano, C 1 -C 6 -alkoxy and C 1 -C 6 -alkylamino;
R is carboxyl;
R″ is selected from hydrido and C 2 -C 6 -alkenyl;
R 1 is selected from C 1 -C 3 -perfluoroalky, chloro, C 1 -C 6 -alkylthio, nitro, cyano and cyano-C 1 -C 3 -alkyl;
R 2 is one or more radicals independently selected from the group consisting of hydrido; halo; C 1 -C 6 -alkyl; C 2 -C 6 -alkenyl; C 2 -C 6 -alkynyl; halo-C 2 -C 6 -alkynyl; pheny-C 1 -C 6 -alkyl; phenyl-C 2 -C 6 -alkynyl; halophenyl-C 2 -C 6 -alkynyl; C 1 -C 6 -alkoxy-phenyl-C 2 -C 6 -alkynyl, phenyl-C 2 -C 6 -alkenyl; C 1 -C 3 -alkoxy; methylenedioxy; C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl; C 1 -C 3 -alkylthio; C 1 -C 3 -alkylsulfinyl; phenyloxy; phenylthio; phenylsulfinyl; C 1 -C 3 -haloalkyl-C 1 -C 3 -hydroxyalkyl; phenyl-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl; C 1 -C 3 -haloalkyl; C 1 -C 3 -haloalkoxy; C 1 -C 3 -haloalkylthio; C 1 -C 3 -hydroxyalkyl; C 1 -C 3 -hydroxyhaloalkyl; hydroxyimino-C 1 -C 3 -alkyl; C 1 -C 6 -alkylamino; nitro; cyano; amino; aminosulfonyl; N—(C 1 -C 6 -alkyl)aminosulfonyl; N-arylaminosulfonyl; N-heteroarylaminosulfonyl; N-(phenyl-C 1 -C 6 -alkyl)aminosulfonyl; N-(heteroaryl-C 1 -C 6 -alkyl)aminosulfonyl; phenyl-C 1 -C 3 -alkylsulfonyl; 5- to 8-membered heterocyclylsulfonyl; C 1 -C 6 -alkylsulfonyl; phenyl; optionally substituted phenyl substituted by one or more radials selected from chloro, fluoro, bromo, methoxy, methylthio and methylsulfonyl; 5- to 9-membered heteroaryl; chloro substituted thienyl; phenyl-C 1 -C 6 -alkylcarbonyl; phenylcarbonyl; 4-chlorophenylcarbonyl; 4-hydroxyphenylcarbonyl; 4-trifluoromethylphenylcarbonyl; 4-methoxyphenylcarbonyl; aminocarbonyl; formyl; and C 1 -C 6 -alkylcarbonyl;
or R 2 together with ring A forms a naphthyl, benzofurylphenyl, or quinolyl radical;
the A ring atoms A 1 , A 2 , and A 3 are carbon and A 4 is carbon or nitrogen; n is an integer selected from 1 to 4;
or a pharmaceutically acceptable salt thereof;
[2] A compound described in [1], wherein
R a is selected from hydrido; methyl; ethyl; (4-trifluoromethyl)benzyl; (4-chloromethyl)benzyl; (4-methoxy)benzyl; (4-cyano)benzyl; and (4-nitro)benzyl;
R″ is selected from hydrido and ethenyl;
R 1 is selected from trifluoromethyl and pentafluoroethyl;
R 2 is one or more radicals independently selected from the group consisting of hydrido; chloro; bromo; fluoro; iodo; methyl; tert-butyl; ethenyl; ethynyl; 5-chloro-1-pentynyl; 1-pentynyl; 3,3-dimethyl-1-butynyl; benzyl; phenylethyl; phenylethynyl; 4-chlorophenyl-ethynyl; 4-methoxyphenyl-ethynyl; phenylethenyl; methoxy; methylthio; methylsulfinyl; phenyloxy; phenylthio; phenylsulfinyl; methylenedioxy; benzyloxymethyl; trifluoromethyl; difluoromethyl; pentafluoroethyl; trifluoromethoxy; trifluoromethylthio; hydroxymethyl; hydroxy-trifluoroethyl; methoxymethyl; hydroxyiminomethyl; N-methylamino; nitro; cyano; amino; aminosulfonyl; N-methylaminosulfonyl; N-phenylaminosulfonyl; N-furylaminosulfonyl; N-(benzyl)aminosulfonyl; N-(furylmethyl)aminosulfonyl; benzylsulfonyl; phenylethylaminosulfonyl; furylsulfonyl; methylsulfonyl; phenyl; phenyl substituted with one or more radicals selected from chloro, fluoro, bromo, methoxy, methylthio and methylsulfonyl; benzimidazolyl; furyl; thienyl; thienyl substituted with chloro; benzylcarbonyl; phenylcarbonyl; aminocarbonyl; formyl; and methylcarbonyl;
or a pharmaceutically acceptable salt thereof;
[3] A compound described in [1] or [2], wherein the compound of formula (I′) is one or more selected from the group consisting of
6-chloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-7-methyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-(1-methylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; (S)-6-chloro-7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-8-(1-methylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 2-trifluoromethyl-3H-naphtopyran-3-carboxylic acid; 7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-bromo-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-chloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-trifluoromethoxy-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; (S)-6-trifluoromethoxy-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 5,7-dichloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-phenyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 7,8-dimethyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6,8-bis(dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 7-(1-methylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 7-phenyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-7-ethyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-8-ethyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-7-phenyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6,7-dichloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6,8-dichloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 2-trifluoromethyl-3H-naphtho[2,1-b]pyran-3-carboxylic acid; 6-chloro-8-methyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-chloro-6-methyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-chloro-6-methoxy-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-bromo-8-chloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-bromo-6-fluoro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-bromo-6-methyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-bromo-5-fluoro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-chloro-8-fluoro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-bromo-8-methoxy-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[[(phenylmethyl)amino]sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[(dimethylamino)sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[(methylamino)sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[(4-morpholino)sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[(1,1-dimethylethyl)aminosulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[(2-methylpropyl)aminosulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-methylsulfonyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-chloro-6-[[(phenylmethyl)amino]sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-phenylacetyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6,8-dibromo-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 8-chloro-5,6-dimethyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; (S)-6,8-dichloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-benzylsulfonyl-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[[N-(2-furylmethyl)amino]sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-[[N-(2-phenylethyl)amino]sulfonyl]-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 6-iodo-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; 7-(1,1-dimethylethyl)-2-pentafluoroethyl-2H-1-benzopyran-3-carboxylic acid; and 6-chloro-2-trifluoromethyl-2H-1-benzothiopyran-3-carboxylic acid;
or a pharmaceutically acceptable salt thereof;
[4] A compound described in any of [1] to [3], wherein the compound of formula (I′) is one or more selected from the group consisting of
6-chloro-8-methyl-2-trifluoromethyl-2H-1-benzothiopyran-3-carboxylic acid; (S)-6-chloro-7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzothiopyran-3-carboxylic acid; (S)-6,8-dichloro-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid; and (S)-6-trifluoromethoxy-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid;
or a pharmaceutically acceptable salt thereof;
[5] A compound described in any of [1] to [4], wherein X is O;
or a pharmaceutically acceptable salt thereof;
[6] A pharmaceutical composition for preventing or treating an ocular disease, wherein the pharmaceutical composition contains a compound as described in any one of [1] to [5] or a pharmaceutically acceptable salt thereof as an active ingredient;
[7] The pharmaceutical composition described in [6], wherein the ocular disease is retinochoroidal degeneration;
[8] The pharmaceutical composition described in [6] or [7], wherein the ocular disease is accompanied with retinochoroidal neovascularization;
[9] The pharmaceutical composition described in [6], wherein the ocular disease is one or more selected from the group consisting of age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof;
[10] A kit for preventing or treating an ocular disease, wherein the kit comprises a compound described in any one of [1] to [5] or a pharmaceutically acceptable salt thereof;
[11] A compound described in any one of [1] to [5] or a pharmaceutically acceptable salt thereof for preventing or treating an ocular disease, wherein the compound has a benzopyran ring or a naphtopyran ring;
[12] A use of a compound as described in any one of [1] to [5] or a pharmaceutically acceptable salt thereof for the manufacture of a medicament for preventing or treating an ocular disease;
[13] The use described in [12], wherein the ocular disease is retinochoroidal degeneration;
[14] The use described in [12], wherein the ocular disease is accompanied with retinochoroidal neovascularization;
[15] The use described in [12], wherein the ocular disease is one or more selected from the group consisting of age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof;
[16] A method for preventing or treating an ocular disease, wherein the method comprises administering an effective amount of a compound described in any one of [1] to [5] to patients;
[17] The method described in [16], wherein the ocular disease is retinochoroidal degeneration;
[18] The method in [16], wherein the ocular disease is accompanied with retinochoroidal neovascularization;
[19] The method described in [16], wherein the ocular disease is one or more selected from the group consisting of age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof; and
[20] A compound as defined by the following formula (I) for use in preventing or treating an ocular disease in animal including human:
[0000]
[0000] wherein
X is selected from O, S and NR a ;
R a is selected from hydrido, C 1 -C 3 -alkyl, (optionally substituted phenyl)-methyl, and phenylmethyl; wherein the phenyl ring is substituted by 1 to 3 substituents independently selected from C 1 -C 6 -alkyl, hydroxyl, halo, C 1 -C 6 -haloalkyl, nitro, cyano, C 1 -C 6 -alkoxy and C 1 -C 6 -alkylamino;
R is carboxyl;
R″ is selected from hydrido and C 2 -C 6 -alkenyl;
R 1 is selected from C 1 -C 3 -perfluoroalky, chloro, C 1 -C 6 -alkylthio, nitro, cyano and cyano-C 1 -C 3 -alkyl;
R 2 is one or more radicals independently selected from hydrido; halo; C 1 -C 6 -alkyl; C 2 -C 6 -alkenyl; C 2 -C 6 -alkynyl; halo-C 2 -C 6 -alkynyl; pheny-C 1 -C 6 -alkyl; phenyl-C 2 -C 6 -alkynyl; phenyl-C 2 -C 6 -alkenyl; C 1 -C 3 -alkoxy; methylenedioxy; C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl; C 1 -C 3 -alkylthio; C 1 -C 3 -alkylsulfinyl; phenyloxy; phenylthio; phenylsulfinyl; C 1 -C 3 -haloalkyl-C 1 -C 3 -hydroxyalkyl; phenyl-C 1 -C 3 -alkoxy-C 1 -C 3 -alkyl; C 1 -C 3 -haloalkyl; C 1 -C 3 -haloalkoxy; C 1 -C 3 -haloalkylthio; C 1 -C 3 -hydroxyalkyl; hydroxyimino-C 1 -C 3 -alkyl; C 1 -C 6 -alkylamino; nitro; cyano; amino; aminosulfonyl; N—(C 1 -C 6 -alkyl)aminosulfonyl; N-arylaminosulfonyl; N-heteroarylaminosulfonyl; N-(phenyl-C 1 -C 6 -alkyl)aminosulfonyl; N-(heteroaryl-C 1 -C 6 -alkyl)aminosulfonyl; phenyl-C 1 -C 3 -alkylsulfonyl; 5- to 8-membered heterocyclylsulfonyl; C 1 -C 6 -alkylsulfonyl; phenyl; optionally substituted phenyl substituted by one or more radials selected from chloro, fluoro, bromo, methoxy, methylthio and methylsulfonyl; 5- to 9-membered heteroaryl; chloro substituted thienyl; phenyl-C 1 -C 6 -alkylcarbonyl; phenylcarbonyl; 4-chlorophenylcarbonyl; 4-hydroxyphenylcarbonyl; 4-trifluoromethylphenylcarbonyl; 4-methoxyphenylcarbonyl; aminocarbonyl; formyl; and C 1 -C 6 -alkylcarbonyl;
the A ring atoms A 1 , A 2 , and A 3 are carbon and A 4 is carbon or nitrogen;
or R 2 together with ring A forms a naphthyl, benzofurylphenyl, or quinolyl radical;
or a pharmaceutically acceptable salt thereof.
Effect of the Invention
[0066] As mentioned above, a lot of COX-2 inhibitors are known, but the third generation COX-2 inhibitors of the present invention, compared to conventional COX-2 inhibitors, show an excellent effect against a chorioretinal neovascularization inhibitory activity. Namely, in evaluation studies of inhibitory activities against a chorioretinal neovascularization, a compound of the present invention completely inhibits events accompanied with a chorioretinal neovascularization to control levels. Therefore, it is particularly useful for preventing or treating an ocular disease accompanied with neovascularization.
[0067] More specifically, a compound of the present invention is useful as a prophylactic and/or therapeutic agent for age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof. In addition, a compound of the present invention is useful for providing a pharmaceutical composition for preventing or treating the said diseases.
BRIEF DESCRIPTION OF THE DRAWINGS
[0068] FIG. 1 shows mean and standard error in evaluation studies of inhibitory activities against retinal neovascularization wherein Compound A is (S)-6-chloro-7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid (n=6). ##:P<0.01, **:P<0.01 (Compound A vs. vehicle in Dunnet's test).
[0069] FIG. 2 shows mean and standard error in evaluation studies of inhibitory activities against retinal neovascularization wherein Compound A is (S)-6-chloro-7-(1,1-dimethylethyl)-2-trifluoromethyl-2H-1-benzopyran-3-carboxylic acid (n=7-11). N.S. means no significant difference. *:P<0.05 (Compound A vs. solvent in Dunnet's test).
[0070] FIG. 3 shows images of histpathological specimens.
DESCRIPTION OF EMBODIMENTS
[0071] Hereafter, definitions of terms and phrases (atoms, groups, rings, etc.) to be used in the present specification will be described in detail. Further, when the other definitions of terms and phrases are applied to the definitions of terms and phrases mentioned below, preferred ranges of the respective definitions and the like can also be applied.
[0072] As used in compounds represented by the formula (I) or the formula (I′), the term “alkyl” as a group or part of a group e.g. alkoxy or hydroxyalkyl refers to a straight or branched alkyl group in all isomeric forms.
[0073] The term “C 1 -C 6 alkyl” refers to an alkyl group, as represented by the formula (I) or the formula (I′), containing at least 1, and at most 6 carbon atoms. Examples of such alkyl groups include methyl, ethyl, propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl and the like.
[0074] The term “C 2 -C 6 alkenyl” refers to an alkenyl group, as represented by the formula (I) or the formula (I′), containing at least 2, and at most 6 carbon atoms. Examples of such alkenyl groups include vinyl, 1-propenyl, allyl, 1-butenyl, 2-butenyl, 3-butenyl, pentenyl, hexenyl and the like.
[0075] The term “C 2 -C 6 alkynyl”, refers to an alkynyl group, as represented by the formula (I) or the formula (I′), containing at least 2, and at most 6 carbon atoms. Examples of such alkynyl groups include ethynyl, 1-propynyl, 2-propynyl, 1-butynyl, 3-butynyl, pentynyl, hexynyl and the like.
[0076] In a compound represented by the formula (I) or the formula (I′), the term “halogen” refers to fluorine (F), chlorine (Cl), bromine (Br), or iodine (I) and the term “halo” refers to the halogen: fluoro (—F), chloro (—Cl), bromo (—Br) and iodo (—I).
[0077] As the term “heteroring” in a heteroaryl, 5- to 8-membered heterocyclyl and 5- to 9-membered heteroaryl in the definition of the formula (I) or the formula (I′), 5- to 6-membered heteroring containing one to three selected from O, N, and S, exemplified by furyl, thienyl, pyridyl, thiazolyl and the like are preferable. These groups may be substituted with conventional substituents such as C 1 -C 6 lower alkyl group, hydroxyl group, amino group, carboxyl group, and halogen. Also, 5- to 8-membered heterocyclyl ring and 5- to 9-membered heteroaryl may be a bicyclic group such as benzimidazolyl.
[0078] In a compound represented by the formula (I) or the formula (I′),
[0000] the term “C 1 -C 6 alkoxy” refers to an alkoxy group containing at least 1, and at most 6 carbon atoms. Examples of such alkoxy groups include methoxy group, ethoxy group, normal propoxy group, isopropoxy group, normal butoxy group, secondary butoxy group, tertiary butoxy group, normal pentyl group, isopentyl group, tertiary pentyl group, neopentyl group, 2,3-dimethylpropyl group, 1-ethylpropyl group, 1-methylbutyloxy group, normal hexyloxy group, isohexyloxy group, 1,1,2-trimethylpropyloxy group and the like;
the term “C 1 -C 6 alkylthio” refers to an alkylthio group containing at least 1, and at most 6 carbon atoms. Examples of such alkylthio groups include methylthio group, ethylthio group, normal propylthio group, isopropylthio group, normal butylthio group, secondary butylthio group, tertiary butylthio group, normal pentylthio group, isopentylthio group, tertiary pentylthio group, neopentylthio group, 2,3-dimethylpropylthio group, 1-ethylpropylthio group, 1-methylbutylthio group, normal hexylthio group, isohexylthio group, 1,1,2-trimethylpropylthio group and the like;
the term “C 1 -C 3 alkylsulfinyl” refers to an alkylsulfinyl group containing at least 1, and at most 6 carbon atoms. Examples of such alkylsulfinyl groups include methylsulfinyl group, ethylsulfinyl group, normal propylsulfinyl group, isopropylsulfinyl group and the like;
the term “C 1 -C 6 alkylsulfonyl” refers to an alkylsulfonyl group containing at least 1, and at most 6 carbon atoms. Examples of such alkylsulfonyl groups include methylsulfonyl group, ethylsulfonyl group, normal propylsulfonyl group, isopropylsulfonyl group, normal butylsulfonyl group, secondary butylsulfonyl group, tertiary butylsulfonyl group, normal pentylsulfonyl group, isopentylsulfonyl group, tertiary pentylsulfonyl group, neopentylsulfonyl group, 2,3-dimethylpropylsulfonyl group, 1-ethylpropylsulfonyl group, 1-methylbutylsulfonyl group, normal hexylsulfonyl group, isohexylsulfonyl group, 1,1,2-trimethylpropylsulfonyl group and the like;
the term “C 1 -C 6 alkylcarbonyl” refers to an alkylcarbonyl group containing at least 1, and at most 6 carbon atoms. Examples of such alkylcarbonyl groups include acetyl group, propanoyl group, butanoyl group, 2-methyl-propanoyl group, pentanoyl group, 2-methylbutanoyl group, 3-methylbutanoyl group and the like; and
the term “C 1 -C 6 alkylamino” refers to an alkylamino group containing at least 1, and at most 6 carbon atoms. Examples of such alkylamino groups include methylamino group, ethylamino group, propylamino group, isopropylamino group, dimethylamino group, diethylamino group, ethylmethylamino group, dipropylamino group, methylpropylamino group, diisopropylamino group and the like.
[0079] For example, the third generation coxib compound represented by formula (I) or formula (I′) is described in Patent Document 1 (Japanese Patent No. 4577534) and the like. A compound of formula (I) or formula (I′) or a salt thereof can be easily prepared by known methods or known methods per se.
[0080] The term “ocular disease” in the present invention refers to, but not limited to, such ocular diseases accompanied with chorioretinal degenerative disease or neovascularization.
[0081] The chorioretinal is an organization combined retina and choroid.
[0082] Examples of an ocular disease accompanied with ocular neovascularization may include, but not limited to, age-related macular degeneration or the like, and therefore, a compound of the present invention is useful as a prophylactic and/or therapeutic agent for age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof.
[0083] The specific diseases are for a better understanding of the invention and are not intended to limit the scope of the invention.
[0084] In terms of pharmaceutically acceptable salts of the compound represented by the formula (I) or the formula (I′), the nature of the salt is not critical, provided that it is pharmaceutically acceptable. Pharmaceutically-acceptable acid addition salts of the compound represented in the formula (I) or the formula (I′) can be prepared from a suitable inorganic acid or from a suitable organic acid. Examples of such inorganic acids are hydrochloric, hydrobromic, hydroiodic, nitric, carbonic, sulfuric and phosphoric acid. Examples of such organic acids are selected from aliphatic, cycloaliphatic, aromatic, araliphatic, heterocyclic, carboxylic and sulfonic classes of organic acids, which are exemplified by formic, acetic, propionic, succinic, glycolic, gluconic, lactic, malic, tartaric, citric, ascorbic, glucuronic, maleic, fumaric, pyruvic, aspartic, glutamic, benzoic, anthranilic, mesylic, salicyclic, salicyclic, 4-hydroxybenzoic, phenylacetic, mandelic, embonic, pamoic, methanesulfonic, ethanesulfonic, benzenesulfonic, pantothenic, 2-hydroxyethanesulfonic, toluenesulfonic, sulfanilic, cyclohexylaminosulfonic, stearic, algenic, β-hydroxybutyric, salicyclic, galactaric, and galacturonic acid. Suitable pharmaceutically-acceptable base addition salts of the compounds represented by the formula (I) or the formula (I′) include metallic salts, such as salts made from aluminum, calcium, lithium, magnesium, potassium, sodium and zinc, or salts made from organic bases including primary, secondary and tertiary amines, substituted amines including cyclic amines, such as caffeine, arginine, diethylamine, N-ethylpiperidine, histidine, glucamine, isopropylamine, lysine, morpholine, N-ethylmorpholine, piperazine, piperidine, triethylamine, and trimethylamine. All salts described above can be prepared from the compound represented by the formula (I) or the formula (I′) and a suitable acid or a suitable base by conventional methods. Then an esterified carboxyl group preferably includes a group capable of converting to a carboxyl group by hydrolysis in vivo (e.g., t-butoxycarbonyl group). Since such groups which can easily converting to a carboxyl group by hydrolysis in vivo are conventionally well established, the present invention may make in accordance with such established known techniques in terms of the type, manufacturing, and the like.
[0085] Compounds of the present invention containing one or more asymmetric carbon atoms can exist as two or more stereoisomers. Where a compound of the present invention contains an alkenyl or alkenylene group, geometric cis/trans (or Z/E) isomers are possible. Where the compound contains, for example, a keto or oxime group or an aromatic moiety, tautomeric isomerism (‘tautomerism’) can occur. It follows that a single compound may exhibit more than one type of isomerism.
[0086] Included within the scope of the present invention are all stereoisomers, geometric isomers and tautomeric forms of the compounds of the present invention, including compounds exhibiting more than/equal to two type of isomerism, and mixtures of one or more thereof. Also included are acid addition salts or base salts wherein the counter ion is optically active, for example, D-lactate or L-lysine, or racemic, for example, DL-tartrate or DL-arginine.
[0087] Cis/trans isomers may be separated by conventional techniques well known to those skilled in the art, for example, chromatography and fractional crystallization.
[0088] Conventional techniques for the preparation/isolation of individual enantiomers include chiral synthesis from a suitable optically pure precursor and resolution of the racemate (or the racemate of a salt or derivative) using, for example, chiral high pressure liquid chromatography (HPLC).
[0089] Alternatively, the racemate (or a racemic precursor) may be reacted with a suitable optically active compound, for example, an alcohol, or, in the case where the compound of the present invention contains an acidic or basic moiety, an acid or base such as tartaric acid or 1-phenylethylamine. The resulting diastereomeric mixture may be separated by chromatography and/or fractional crystallization and one or both of the diastereoisomers can be converted to the corresponding pure enantiomer(s) by means well known to a skilled person.
[0090] Chiral compounds of the present invention (and chiral precursors thereof) may be obtained in enantiomerically-enriched form using chromatography, typically HPLC, on an asymmetric resin with a mobile phase containing alcohol from 0 to 50 (w/w) %, typically ethanol and 2-propanol from 2 to 20 (w/w) %, and carboxylic acid from 0 to 5 (w/w) %, typically hydrocarbon including acetic acid from 0.1 to 0.5 (w/w) %, typically heptane or hexane. Concentration of the eluate affords the enriched mixture.
[0091] More specifically, heptane/2-propanol/trifluoroacetic acid (95/5/0.1), heptane/2-propanol/acetic acid (90/10/0.1), heptane/2-propanol/acetate (90/10/0.5), heptane/ethanol/acetic acid (95/5/0.1) or the like may be used for the said mobile phase.
[0092] Stereoisomeric conglomerates may be separated by conventional techniques known to those skilled in the art—see, for example, Stereochemistry of Organic Compounds by E L Eliel (Wiley, New York, 1994).
[0093] The present invention includes all pharmaceutically acceptable isotopically-labeled compounds of the present invention wherein one or more atoms are replaced by atoms having the same atomic number, but an atomic mass or mass number different from the atomic mass or mass number usually found in nature.
[0094] Examples of isotopes suitable for inclusion in the compounds of the present invention include isotopes of hydrogen such as 2 H and 3 H, carbon such as 11 C, 13 C and 14 C, chlorine such as 38 Cl, fluorine such as 18 F, iodine such as 123 I and 125 I, nitrogen such as 13 N and 15 N, oxygen such as 15 O, 17 O and 18 O, phosphorus such as 32 P, and sulfur such as 35 S.
[0095] Certain isotopically-labeled compounds of the present invention, for example, those incorporating a radioactive isotope, are useful in drug and/or substrate tissue distribution studies associated with cancer therapy which includes diagnosis, alleviation of symptoms, improvement of QOL, and prophylaxis. The radioactive isotopes tritium, i.e. 3 H, and carbon-14, i.e. 14 C, are particularly useful for this purpose in view of their ease of incorporation and ready means of detection.
[0096] Substitution with heavier isotopes such as deuterium, i.e. 2 H, may afford certain therapeutic advantages resulting from greater metabolic stability, for example, increased in vivo half-life or reduced dosage requirements, and hence may be preferred in some circumstances.
[0097] Substitution with positron emitting isotopes, such as 11 C, 18 F, 15 O and 13 N, can be useful in Positron Emission Topography (PET) studies for examining substrate receptor occupancy.
[0098] Isotopically-labeled compounds of the present invention can generally be prepared by conventional techniques known to those skilled in the art or by processes analogous to those described in the accompanying Examples and Preparations using an appropriate isotopically-labeled reagent in place of the non-labeled reagent previously employed.
[0099] Pharmaceutically acceptable solvates in accordance with the present invention include those wherein the solvent for crystallization may be isotopically substituted, e.g., D 2 O, d 6 -acetone, and d 6 -DMSO.
[0100] Compounds of the present invention intended for pharmaceutical use may be administered as crystalline or amorphous products. They may be obtained, for example, as solid plugs, powders, or films by methods such as precipitation, crystallization, freeze drying, spray drying, and evaporative drying. Microwave or radio frequency drying may be used for this purpose.
[0101] A compound of the present invention exhibits an excellent effect on HUVEC (Human Umbilical Vein Endothelial Cells) lumen formation study, VEGF (vascular endothelial growth factor)-induced human retinal microvascular endothelial cell (HRMEC) proliferation study, and VEGF-induced HRMEC migration study as in vivo evaluation studies of inhibitory activities against retinal neovascularization.
[0102] In a mouse model of choroidal neovascularization induced by krypton laser irradiation and a model of hyperoxia-induced retinal neovascularization as in vivo studies, a compound of the present invention exhibits an excellent inhibitory effect on choroidal neovascularization through intravitreal administration.
[0103] Incidentally, this model is considered to be a model of an ocular inflammatory disease and/or a model of a retinal disease typified by age-related macular degeneration or the like, and therefore, a compound of the present invention is useful as a prophylactic and/or therapeutic agent for age-related macular degeneration, retinopathy of prematurity, polypoidal choroidal vasculopathy, diabetic retinopathy, diabetic macular edema, ischemic proliferative retinopathy, retinitis pigmentosa, cone dystrophy, proliferative vitreoretinopathy, retinal artery occlusion, retinal vein occlusion, keratitis, conjunctivitis, uveitis, Leber's disease, retinal detachment, retinal pigment epithelial detachment, neovascular glaucoma, corneal neovascularization, retinochoroidal neovascularization and an ocular disease accompanied with the diseases thereof.
[0104] The present compound can be administered orally or parenterally. Examples of the mode of administration include oral administration, ophthalmic topical administration (such as eye drop administration, instillation in the conjunctivalsac, intravitreal administration, subconjunctival administration and sub-Tenon's administration), intravenous administration and transdermal administration, and the present compound can be formulated into a preparation suitable for such an administration mode by properly selecting and using a pharmaceutically acceptable additive as needed.
[0105] Examples of the dosage form include, in the case of an oral preparation, a tablet, a capsule, a granule and a powder, and, in the case of a parenteral preparation, an injection, an eye drop, an eye ointment, an insert and an intraocular implant.
[0106] For example, in the case of a tablet, a capsule, a granule, a powder or the like, such a preparation can be prepared by properly selecting and using an excipient such as lactose, glucose, D-mannitol, anhydrous calcium hydrogen phosphate, starch or sucrose; a disintegrant such as carboxymethyl cellulose, calcium carboxymethyl cellulose, croscarmellose sodium, crosspovidone, starch, partially gelatinized starch or low-substituted hydroxypropyl cellulose; a binder such as hydroxypropyl cellulose, ethyl cellulose, gum arabic, starch, partially gelatinized starch, polyvinylpyrrolidone or polyvinyl alcohol; a lubricant such as magnesium stearate, calcium stearate, talc, hydrous silicon dioxide or a hydrogenated oil; a coating agent such as purified sucrose, hydroxypropylmethyl cellulose, hydroxypropyl cellulose, methyl cellulose, ethyl cellulose or polyvinylpyrrolidone; a corrigent such as citric acid, aspartame, ascorbic acid or menthol; or the like as needed.
[0107] An injection can be prepared by properly selecting and using a tonicity agent such as sodium chloride; a buffer such as sodium phosphate; a surfactant such as polyoxyethylene sorbitan monoolate; a viscosity-increasing agent such as methyl cellulose; or the like as needed.
[0108] An eye drop can be prepared by properly selecting and using a tonicity agent such as sodium chloride or concentrated glycerin; a buffer such as sodium phosphate or sodium acetate; a surfactant such as polyoxyethylene sorbitan monoolate, polyoxyl 40 stearate or polyoxyethylene hydrogenated castor oil; a stabilizer such as sodium citrate or sodium edetate; a preservative such as benzalkonium chloride or paraben; or the like as needed. The pH of the eye drop is permitted as long as it falls within the range that is acceptable as an ophthalmic preparation, but is preferably in the range of from 4 to 8, and more preferably in the range of from 5 to 7. As a pH adjusting agent, a normal pH adjusting agent, for example, sodium hydroxide and/or hydrochloric acid may be used.
[0109] The material of the resinous container consists essentially of polyethylene. The container material may contain minor amounts of other materials than polyethylene, for example polypropylene, polyethylene terephthalate, polyvinyl chloride, acrylic resins, polystyrene, polymethyl methacrylate and nylon 6. The amount of said materials is preferably no more than about 5 to 10% of the total container material. Polyethylene is classified to several types by the density thereof, namely low density polyethylene (LDPE), middle density polyethylene (MDPE), high density polyethylene (HDPE), etc and these polyethylenes are included in this invention. Preferable polyethylene is LDPE.
[0110] Containers for packaging and storing the aqueous ophthalmic solution according to the invention include all container forms suitable for user-friendly topical ophthalmic delivery. Consequently, the containers may be selected for example from the group consisting of bottles, tubes, ampoules, pipettes and fluid dispensers, in single unit dose form or in multidose form. According to a preferred embodiment of the invention, the aqueous ophthalmic solution is in a single dose or unit dose form.
[0111] The containers for the ophthalmic solution according to the invention are preferably manufactured by extrusion blow moulding method. Extrusion blow moulding gives smoother inner surface of the container compared to injection blow moulding, which is commonly used to manufacture for example polyethylene multidose bottles. The smoother inner surface gives better chemical stability of prostaglandins in the polyethylene container compared to polyethylene container manufactured by injection blow moulding. Furthermore, when single-dose containers are used, they are sterilized during the moulding process by heat and no additional sterilization of containers is needed, which also improves stability of prostaglandins in a single-dose container (see EP 1 825 855 and EP 1 349 580). In general, a unit dose ophthalmic container manufactured by blow moulding method has a volume of about 1 ml and about 0.2 to 0.5 ml of solution is filled. A large variety of shapes are known in such containers. Typical examples are seen in U.S. Pat. No. 5,409,125 and U.S. Pat. No. 6,241,124.
[0112] Although unit dose containers are preferred for the purposes of the invention, the aqueous ophthalmic solution according to the invention remains soluble, stable and bioavailable also in fluid dispensers for dispensing of minute amounts of germ-free fluid or in any other container-type wherein the aqueous ophthalmic solution is in contact with container material consisting essentially of polyethylene. Such fluid dispensers are disclosed for example in U.S. Pat. No. 5,614,172.
[0113] The preservative-free aqueous ophthalmic solution according to the invention can be stored at room temperature in the above mentioned suitable containers, including unit dose pipettes and dispensers.
[0114] A preferred embodiment according to the invention is an aqueous ophthalmic solution for treating ocular hypertension and glaucoma, which comprises 0.0001-0.01% w/v of a compound of formula (I) or formula (I′), or a pharmaceutically acceptable salt thereof as an active ingredient;
[0000] 0.05-0.5% w/v non-ionic surfactant;
0.005-0.2% w/v stabilizing agent;
substantially no preservatives, and optionally buffering agents, pH adjusters and tonicity agents conventionally used in ophthalmic solutions, in a container consisting essentially of polyethylene.
[0115] An eye ointment can be prepared using a widely used base such as white petrolatum or liquid paraffin.
[0116] An insert can be prepared using a biodegradable polymer such as hydroxypropyl cellulose, hydroxypropylmethyl cellulose, a carboxy vinyl polymer or polyacrylic acid, and if necessary, an excipient, a binder, a stabilizer, a pH adjusting agent or the like can be properly selected and used as appropriate.
[0117] A preparation for intraocular implant can be prepared using a biodegradable polymer such as polylactic acid, polyglycolic acid, a lactic acid-glycolic acid copolymer or hydroxypropyl cellulose, and if necessary, an excipient, a binder, a stabilizer, a pH adjusting agent or the like can be properly selected and used as appropriate.
[0118] The dose of the present compound can be properly selected depending on the dosage form, symptoms, age, body weight of a patient or the like. For example, in the case of oral administration, it can be administered in an amount of from 0.01 to 5000 mg, preferably from 0.1 to 2500 mg, particularly preferably from 0.5 to 1000 mg per day in a single dose or several divided doses. In the case of an injection, it can be administered in an amount of from 0.00001 to 2000 mg, preferably from 0.0001 to 1500 mg, particularly preferably from 0.001 to 500 mg per day in a single dose or several divided doses. In the case of an eye drop, a preparation containing the present compound at a concentration of from 0.00001 to 10% (w/v), preferably from 0.0001 to 5% (w/v), particularly preferably from 0.001 to 1% (w/v) can be instilled into the eye once or several times a day. In the case of an eye ointment, a preparation containing the present compound in an amount of from 0.0001 to 2000 mg can be applied. In the case of an insert or a preparation for intraocular implant, a preparation containing the present compound in an amount of from 0.0001 to 2000 mg can be inserted or implanted.
[0119] The present invention also relates to combining separate pharmaceutical compositions in kit form. The kit comprises a container for containing the separate compositions such as a divided bottle or a divided foil packet, however, the separate compositions may also be contained within a single, undivided container. The kit form is particularly advantageous when the separate components are preferably administered in different dosage forms (e.g., oral and parenteral), are administered at different dosage intervals, or when titration of the individual components of the combination is desired by the prescribing physician.
[0120] An example of such a kit is a so-called blister pack. Blister packs are well known in the packaging industry and are being widely used for the packaging of pharmaceutical unit dosage forms (tablets, capsules, and the like). Blister packs generally consist of a sheet of relatively stiff material covered with a foil of a preferably transparent plastic material. During the packaging process, recesses are formed in the plastic foil. The recesses have the size and shape of the tablets or capsules to be packed. Next, the tablets or capsules are placed in the recesses and the sheet of relatively stiff material is sealed against the plastic foil at the face of the foil which is opposite from the direction in which the recesses were formed. As a result, the tablets or capsules are sealed in the recesses between the plastic foil and the sheet. Preferably, the strength of the sheet is such that the tablets or capsules can be removed from the blister pack by manually applying pressure on the recesses whereby an opening is formed in the sheet at the place of the recess. The tablet or capsule can then be removed via said opening.
[0121] A kit product, prefilled syringe, which comes prefilled with desired medicament in a syringe container, can be provided.
Example
[0122] The present invention is explained in more detail in the following by referring to Reference Examples and Examples, which are not to be construed as limitative but just typical examples.
[0123] A compound of formula (I) or formula (I′) can be prepared using any method known in the art (for example, patent literature 1, JP Patent No. P4577534).
[0124] Examples of an ocular disease model accompanied with neovascularization include the following studies.
Evaluation Studies of Inhibitory Activities Against Neovascularization
HUVEC Tube Formation Study
[0125] In co-culture system of human fibroblasts and human umbilical vein endothelial cells (HUVEC), the effect of the drug on the promotion of the HUVEC tube formation by adding VEGF-A is studied. A drug to be evaluated is added to the VEGF-A-added medium. The cultured cells are immobilized after a certain period of time, and the HUVEC stained with an anti-CD31 antibody is subject to morphological observation, and then tube area, total length of tube network, number of branch points, number of branch and the like are evaluated. Journal of Pharmacological Sciences, 129, 451-456 (2007).
VEGF-Induced Human Retinal Microvascular Endothelial Cells (HRMEC) Proliferation Study
[0126] VEGF is a factor which promotes neovascularization and is thought to be one of the causes of development or progression of age-related macular degeneration (Prog. Retinal Eye Res., 22 (1), 1-29 (2003)). Therefore, the inhibitory effect of the compounds of the invention against VEGF-induced cell proliferation is assessed by using human retinal vascular endothelial cells (HRMEC).
[0127] HRMEC are seeded in 96-well plates at 2.0×10 3 cells/well, and is cultured under the conditions of 5% CO 2 /95% air for 24 hours. Then the culture medium is exchanged with CSC medium containing 10% fetal bovine serum and the cells are cultured for 24 hours. The culture broth is exchanged with vehicle medium or study medium containing the compound of the invention at 0.1, 1.0, 10, or 100 microM. After preincubation for 1 hour, VEGF-A solution is added to be a concentration of 10 ng/ml, and the cells cultured for 24 hours. The culture broth without adding VEGF-A solution is also treated in the same manner. Then to the culture broth is added CCK-8, and the cells are cultured for 3 hours, then the absorbance (OD492) is measured.
[0128] In accordance with the following formula, the cell proliferation inhibition rate (%) of each compound-treated group is calculated. The number of examples of each group is six.
[0000] Cell proliferation inhibition rate(%)=(( B X −B N )/( B O −B N ))×100 [equation]
[0000] B O : absorbance of vehicle-treated group
B X : absorbance of compound-treated group
B N : absorbance of non-treated group
[0129] The result of Compound A is shown in FIG. 1 . Although addition of Compound A alone has no effect on the proliferation of HRMEC (on the left side in FIG. 1 ), a compound of the invention inhibits the proliferation of HRMEC induced by VEGF-A in a dose-dependent manner (on the right side in FIG. 1 ). Compound A inhibits the cell proliferation to control levels at 10 to 100 microM.
VEGF-Induced Human Retinal Microvascular Endothelial Cells (HRMEC) Migration Study
[0130] The effects of the drug on the migration of human retinal microvascular endothelial cells (HRMEC) are studied.
[0131] HRMEC are seeded in a 12-well plate coated with collagen at a density of 4×10 4 cells/well, and is cultured at 37° C. under 5% CO 2 for 48 hours. Then after the medium is exchanged with the medium without the growth factors, the cells are cultured for 24 hours. Then, the cells present on the center line of the well scratched by using a 1 mL tip, and medium is exchanged by washing the well with PBS (phosphate buffer solution). Immediately after that, image of HRMEC is recorded by using a CCD camera (pre-migration). VEGF-A and a compound of the present invention are added to the well to attain the target concentration, and the cells are incubated for 24 hours. After migration, each well is recorded in a similar manner, and the number of cells migrated to the place where the cells are scratched is measured comparing with that before migration.
[0132] By addition of VEGF-A, the number of migrated cell of HRMEC increased compared with that of the control group. A significant inhibitory effect on the migration of VEGF-induced HRMEC by addition of the compound of the present invention is observed.
Laser-Induced Choroidal Neovascularization (CNV) Model
[0133] A male C57BL/6J mouse is used. Mydrin P ophthalmic solution (registered trademark, Santen Pharmaceutical) is instilled into the right eye of the mouse to cause mydriasis. Animals are anesthetized, and laser irradiation is performed on around the circumference of the optic disk with eight equally space using a laser photocoagulation apparatus.
[0134] After photocoagulation, intravitreal administration of drugs to the right eye (administering 2 microL of a solution of 60 microM and 600 microM using a solvent obtained by mixing 0.1N NaOH and pH 7.2 PBS containing 1.5×10 −3 N HCl, at the ratio of 16:84) or oral administration/subcutaneous administration/intraperitoneal administration is conducted. After instillation of Cravit (registered trademark, Daiichi Sankyo) ophthalmic solution 0.5% into the right eye, the ocular fundus photography is promptly performed using an ocular fundus camera. On day 7 and day 14 after laser radiation, 10-fold diluted Fluorescite (registered trademark, Nippon Alcon) Intravenus Injection is injected into the tail vein of the anesthetized animal, and the ocular fluorescein fundus angiography is promptly performed using an ocular fundus camera.
[0135] On day 15 after after laser radiation, fluorescein-conjugated dextran (FITC-dextran) is injected into the tail vein of the anesthetized animal. After securing the eyeball excised from the animals, fixed, and a choroidal flat mount specimen is prepared under the microscope. Choroidal flat mounts specimens are observed using a confocal laser scanning microscope, and the CNV area of the image is calculated using the analysis software OLYMPUS FLUOVIEW FV1000.
[0136] The result of Compound A is shown in FIG. 2 . CNV area is significantly reduced in comparison to the vehicle-treated group.
[0137] The pathological image of Compound A is shown in FIG. 3 . CNV area is significantly reduced in comparison to the vehicle-treated group.
Hyperoxia-Induced Retinal Neovascularization (Oxygen-Induced Retinopathy: OIR) Model
[0138] Experiments are carried out according to the method described in Journal of Pharmacological Sciences, 129, 451-456 (2007) and Invest Ophthamol Vis Sci. 1994; 35; p. 101-111. C57BL/6J mice are used. Hyperoxia-induced mouse model is carried out according to Smith's method (Smith L E et al., Invest Ophthamol Vis Sci. 1994; 35; p. 101-111). Newborn mouse is housed along with the parent mouse in high oxygen (75% O 2 ) in the cage, which is controlled by the oxygen control device from postnatal day 7 to postnatal day 12. On postnatal day 12, newborn mouse is back to atmospheric pressure conditions (21% O 2 ), and intravitreal administration of drugs to the right eye (administering 2 microL of a solution of 60 microM and 600 microM using a solvent obtained by mixing 0.1N NaOH and pH 7.2 PBS containing 1.5×10 −3 N HCl, at the ratio of 16:84) or oral administration/subcutaneous administration/intraperitoneal administration is conducted and is housed up to postnatal day 17. Mice are anesthetized in the evaluation period, and FITC-dextran is administered from the left ventricle. After securing the eyeball excised from the animals, fixed, and a choroidal flat mount specimen is prepared under the microscope. Choroidal flat mount specimens are observed using a confocal laser scanning microscope, and the CNV area of the image is calculated using the analysis software OLYMPUS FLUOVIEW FV1000.
[0139] CNV area is significantly reduced by administering a compound of the present invention in comparison to the vehicle-treated group. | The purpose of this invention is to provide a compound for preventing or treating an ocular disease and a pharmaceutical composition comprising the same. This invention provides a pharmaceutical composition comprising a compound as defined by the formula (I′) or a pharmaceutically acceptable salt thereof. The pharmaceutical composition is useful for preventing or treating an ocular disease such as retinochoroidal degeneration. | 2 |
This application is a Continuation in Part of application Ser. No. 10/264,206, “Dual glucose-hydroxybutyrate analytical sensors” filed Oct. 3, 2002 now U.S. Pat. No. 6,984,307, which also claimed priority benefit of provisional patent application 60/327,535 “Dual glucose-hydroxybutyrate analytical sensors”, filed Oct. 5, 2001.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The field of the invention is improved dry reagents for instrumented whole blood tests useful for diabetics.
2. Description of the Related Art
Blood glucose monitoring has revolutionized the treatment of diabetes. Large-scale clinical trials have demonstrated that frequent blood glucose monitoring can aid in the prevention of many of the long-term complications of diabetes, such as diabetic retinopathy, circulatory disorders, and death. After nearly twenty years of development, blood glucose monitoring has now become a several billion dollar a year business.
As the blood glucose-monitoring field has advanced, the various blood glucose monitors have become more and more generic. All possess good accuracy, ease of use, and speed. As a result, the various manufacturers of blood glucose monitors have focused major efforts on gaining minor technical advantages to make minor improvements in their respective market shares. Such improvements may include minor improvements in speed, blood sample size, ease of sample application, cost, etc. All, however, produce test strips that measure only blood glucose.
Although blood glucose is the most important biochemical parameter to measure in diabetes, it is not the only parameter of medical interest. Other parameters of medical relevance include glycosylated hemoglobin, used to measure long-term blood glucose control, ketone levels, used to indicate if the patient is at risk for diabetic ketoacidosis, and lipids such as cholesterol, triglycerides, lipoproteins, and chylomicrons, used to indicate the patient's relative risk of cardiovascular disease.
In this document, ketoacidosis and elevated triglycerides will be used as the main examples of other biochemical parameters that are medically relevant to the treatment of diabetes, however it should be understood that the methods discussed here are general purpose, and may be used for a wide variety of different analytes.
Diabetic ketoacidosis is a major complication of diabetes. Such conditions occur during times of extreme insulin deficiency. Here the diabetic's tissues are unable to process glucose, and as a result, initiate the biochemical processes that result in the formation of ketones and excess blood glucose. During periods of insulin starvation, body cells are unable to metabolize glucose as an energy source and instead metabolize fat as an energy source. Ketone bodies, made up of acectoacetate, acetone, and beta-hydroxybutyrate (also called D-3-hydoxybutyrate) are produced from this fat metabolism process, and these build up in the blood. Excessive levels of ketone bodies in turn can alter the pH balance of the blood to a more acidic state, as well as other undesirable complications, eventually leading to confusion, coma, and death. In the early stages of fat metabolism, the ketone bodies contain relatively large amounts of acectoacetate and acetone. However in more profound ketoacidosis, the ketone bodies contain primarily beta-hydroxybutyrate.
Each year, about 12 out of every 1000 diabetics are hospitalized for Ketoacidosis, and 2% of those hospitalized die from it. It is the commonest cause of death for diabetic children.
Early detection is the best way to prevent diabetic ketoacidosis. If detected in time, rehydration and low-dose insulin therapy can be used to treat ketoacidosis. Thus means to ensure that the onset of ketoacidosis is promptly detected are of extreme utility to diabetics.
Although ketoacidosis is a major problem, the biggest complication of diabetes is cardiovascular disease. Two out of three diabetics ultimately die from heart disease and stroke (caused by cardiovascular disease), and many others suffer from other cardiovascular disease complications such as diabetic retinopathy. Much of this cardiovascular disease in turn is caused by the build-up of fatty deposits (lipid rich plaque) in blood vessels and arteries.
Diabetics, and in particular type 2 diabetics, often have an abnormally large increase in the amount of triglycerides, lipids, and lipoproteins circulating in the blood after meals. This increase is particularly severe for type 2 diabetics who have just eaten meals with a high fat content. This post-meal lipoprotein increase is often referred to as “postprandial lipemia” In postprandial lipemia, a large number of triglyceride-rich chylomicrons, low-density lipoproteins (LDL), very low-density lipoproteins (VLDL) and other lipoproteins are released from the small intestine. These triglyceride-rich chylomicrons and other lipoproteins scatter light, and often cause the plasma and serum from postprandial subjects to have so much optical turbidity that this turbidity interferes with the optical determination of other analytes. As a result, for many clinical analytes, it is a routine clinical practice to require patients to fast for at least twelve hours before providing blood samples.
Recent studies have shown that this postprandial lipemia can do more harm than just generate turbid plasma. The LDL and chylomicron lipoprotein particles tend to build up on the walls of arteries, leading to atherosclerosis (fat deposits on artery walls) and subsequent increased risk of coronary artery disease, stroke, and other cardiovascular disorders.
Fortunately the choice between a high-fat diet that causes substantial postprandial lipemia, and a low-fat diet that avoids high postprandial lipemia, is a relatively easy choice to implement—substitute low-fat foods for high-fat foods. If type 2 diabetics, who are at a particularly high risk for atherosclerosis and other cardiovascular complications caused by postprandial lipemia, and who are accustomed to routinely testing postprandial blood glucose levels, also had a simple way of determining their relative level of postprandial lipemia at the same time, they would be constantly reinforced to chose low-fat diets, and thus could substantially reduce their risk of cardiovascular disease.
Returning to the ketoacidosis example, means to measure ketone levels are known in the art. These include visually read test strips for acetone or acectoacetate in the urine, as well as whole blood tests for beta-hydroxybutyrate. Diabetics are trained that whenever their glucose levels are high, they should follow up by immediately running a separate ketone test.
Examples of urine ketone dry reagent tests include Ketostix, Keto-Diastix (Beyer) or Chemstrip K (Roche). Such urinary tests generally use non-enzymatic detection methods (such as nitroprusside based chemistries) that are primarily sensitive to acectoacetate, slightly sensitive to acetone, and not at all sensitive to beta-hydroxybutyrate. One drawback of tests that measure only urinary acectoacetate or acetone is that such tests can miss or underreport extreme levels of ketoacidosis. In mild ketosis, the body produces acectoacetate, acetone and beta-hydroxybutyrate in relatively proportionate amounts, and thus urinary tests for acectoacetate and acetone will detect mild ketosis. However in extreme ketoacidosis, the body produces mostly beta-hydroxybutyrate and relatively small amounts of acectoacetate and acetone. Thus non-enzymatic nitroprusside based acectoacetate and acetone sensitive tests may become insensitive to extreme ketoacidosis right when they are needed the most.
Simple dry reagent whole blood tests for beta-hydroxybutyrate, the most clinically relevant indicator of ketoacidosis, are known in the art. Presently, such dry reagent tests use a disposable reagent that performs only the beta-hydroxybutyrate test. Often this disposable beta-hydroxybutyrate reagent is read in a meter that is capable of reading a number of different types of single test reagents. For example, GDS diagnostics, Elkhart Ind., sells the “Stat-Site™” meter, which can read separate calorimetric dry reagent tests for either whole blood glucose or ketones (beta-hydroxybutyrate). This technology is taught in U.S. Pat. No. 5,139,685. Polymer Technology Systems of Indianapolis Ind. sells the Bioscanner™ meter that can also read separate calorimetric dry reagent tests for either whole blood glucose or ketones. Similarly, MediSense sells the “Precision Xtra™” meter that can read separate electrochemical dry reagent tests for either glucose or beta-hydroxybutyrate.
Other one-meter multiple-reagents systems are in commercial use. The LXN Corporation sells the “Duet™” and “In Charge System™” meters that are capable of reading either a calorimetric glucose dry reagent test, or alternatively a colorimetric glycated protein (fructosamine) dry reagent test. These are discussed in more detail in U.S. Pat. Nos. 5,695,949 and 6,027,692.
Although diabetics are accustomed to testing their blood glucose several times a day, they may often forget to run a ketone test, since such tests require extra reagents and effort. Indeed, in an effort to correct for this normal human lapse, some glucose meters, such as the LifeScan “ultra” blood glucose system, will attempt to remind users to run ketone tests by an extra “Ketones?” meter prompt. However, clearly many diabetics will ignore this reminder.
Returning to the lipemia example, methods to measure postprandial lipemia are also known in the art. These tests include standard enzymatic tests for triglycerides, lipoprotein precipitation tests using chemical agents that selectively precipitate lipoproteins from plasma, and immunoprecipitation tests for specific lipoproteins (using specific anti-lipoprotein antibodies). Studies have also shown that there is a good correlation between the amount (level, concentration) of plasma or serum chylomicrons and the turbidity (light scattering) of the plasma or serum. Tazuma et. al. (“A quantitative assessment of serum chylomicron by light scattering intensity: Application to the intestinal fat absorption test”, Journal of Gastroenterology and Hepatology, Volume 12(11), November 1997, pp 713-718) utilized this correlation to devise a clinical test for serum chylomicrons based on light scattering nephelometric, (turbidimetric) methods. Tazuma et. al. found that a linear relationship existed between serum light scattering (using serum diluted 1:10 into 0.9% saline) and triglyceride concentration. Specifically, in Tazuma's system, this relationship was shown by equation 1 below:
y= 0.33[ x]+ 14.969 x Equation 1
Here “y” is the serum chylomicron triglyceride concentration (level) in mg/dl, and “x” is the relative extent of plasma light scattering on Tazuma's Nippon Shoji Micronephelometer MN-202, used for this experiment.
Although Tazuma's work shows that it is possible to use light scattering measurements to determine triglyceride levels in diluted serum, this is an unusual approach that has not previously been used for whole blood dry reagent tests. More typically, whole blood triglyceride dry reagent tests are based upon enzymatic reactions that produce a colored reaction product and are measured by a calorimetric instrument. Examples of this type of test include the Polymer Technology Systems (Indianapolis, Ind.) “Cardiocheck” system, and the Polymer Technology Systems “Lipid Panel” test strips. The “Lipid Panel” test strips measure total cholesterol, HDL (high density lipoprotein), and triglycerides using plasma obtained from whole blood by filtering the blood through a spreading layer, a blood separation layer, and a fractionation layer. The resulting purified plasma is then read in three separate enzymatic reaction zones, each zone containing a different enzymatic chemistry that generates a colorimetric reaction.
The Cholestech LDX analyzer (Cholestech corporation, Hayward, Calif.), exemplified by U.S. Pat. Nos. 5,110,724; 5,114,350 and 5,171,688 is another dry reagent triglycerides test that also measures total cholesterol, HDL, and triglycerides by a similar process in which whole blood is first fractionated into plasma, and then read in three separate enzymatically based calorimetric reaction pads. Due to the need to separate whole blood into plasma prior to contact with the various enzymatic reaction zones, both systems require relatively large amounts of blood and both systems are relatively slow The PTS Lipid panel test requires 40 ul of blood and requires two minutes to perform a test. The Cholestech LDX system requires approximately 60 ul of blood and requires about five minutes to perform a test. As a result, neither approach would be competitive in the blood glucose market, where sample sizes are invariably less than 20 ul, and test times are often only a few seconds are less.
Ideally, what is best from a medical perspective is a blood glucose test that automatically (without any extra user thought, process, or intervention) also reports blood beta-hydroxybutyrate levels, or blood lipid (triglyceride or chylomicron) levels, or other important second analyte levels, using the same drop of blood used to perform the standard and habitual glucose test. Indeed such a combined test would save many lives by facilitating the early detection of ketoacidosis, prevention of atherosclerosis, or other complication of diabetes. Additionally, such combined tests would be of strong commercial interest as well, since if everything else were equal, a combined glucose/beta-hydroxybutyrate test, glucose/triglycerides test, glucose/lipoprotein test, glucose/chylomicron test, or glucose/relevant-second-analyte test would be strongly preferred by diabetics over the glucose-only tests presently used.
However no such single-blood-drop-activated, combined blood-glucose/blood-beta-hydroxybutyrate dry reagent or combined glucose/lipoprotein reagent has previously been proposed, invented, or commercialized.
By contrast, combined glucose-ketone test strips have been available for urine testing for many years. Given the competitive nature of the blood glucose-monitoring field, why does this discrepancy exist between the long-term commercialization of combined urine glucose-ketone dry reagent test strips, and the complete lack of any prior art in combined high speed, low blood sample, whole blood glucose/beta-hydroxybutyrate or blood glucose-second analyte dry reagent tests?
The difference is almost certainly due to the radically different nature of the two different sample types. Urine is available in large (100+ milliliter [ml]) quantities. It is nearly transparent. Thus a combined glucose-ketone dry regent test may be made by simply putting a calorimetric glucose dry reagent test pad onto solid support a certain distance away from a colorimetric ketone dry regent test pad. Because large amounts of sample are present, the distance between the two test pads can be so great as to minimize any “cross talk” due to reaction intermediate or colorimetric dye indicator diffusion between the two pads.
It is often the case in nearly every area of technology that devices optimized for a single purpose outperform devices optimized for multiple purposes. Blood glucose testing has been a mature field for nearly twenty years, and blood glucose meters and reagents have evolved to a highly advanced state. Patients and physicians are unlikely to accept a dual glucose-beta-hydroxybutyrate or glucose-lipemia reagent as being a genuine improvement unless, at a minimum, the glucose portion of the reagent performs at a level that is competitive with stand-alone blood glucose tests. If the combined reagent requires no extra user effort, the blood glucose portion is competitive, and the extra cost for the secondary function is minor, then the user will benefit and the combined reagent will likely be a medical and commercial success.
In this context, the commercial success of combined urine-ketone test strips can be understood. These devices function with the same urine sample and require no additional user effort. The urine glucose part of a combined urinary glucose-ketone test strip performs as well as stand-alone urine glucose test strip.
By contrast, combined whole blood glucose-beta-hydroxybutyrate or other relevant glucose-second analyte dry reagents must overcome some formidable technical challenges. Whereas urine samples typically have a volume of 100 ml (milliliters), blood samples, typically derived from a fingerstick, are more typically have a volume around 1-10 ul (microliters), or more generally from about 0-20 ul. This is nearly five orders of magnitude less in size. Whereas urine is nearly transparent and relatively free of optical and electrochemical interfering substances, blood is intensely colored and contains nearly 50% hemoglobin and other strong optical and electrochemical interfering substances.
In order to meet the requirement for no additional user effort, a whole blood combined glucose-ketone/beta-hydroxybutyrate or other relevant glucose-second analyte test must place both the glucose sensing means and the ketone/beta-hydroxybutyrate (or other second analyte sensing means) close enough together as to both be activated with the same small (1-10 ul, or 0-20 ul) drop of whole blood. Further, the test must be designed to minimize “cross talk” between such closely spaced sensing means.
PRIOR ART
Visually read beta-hydroxybutyrate sensors and ketone sensors.
U.S. Pat. No. 4,147,514 teaches a urine test strip for detecting urinary acetone and acetoacetic acid by means of an improved nitroprusside reaction. This urinary ketone test strip patent, in conjunction with U.S. Pat. No. 3,814,668 for a urinary glucose test strip, forms the basis for the popular Keto-Diastix® Reagent strips for urinalysis, produced by Bayer Corporation, Elkhart Ind.
U.S. Pat. No. 4,397,956 teaches a whole-blood modification of the combined urine glucose-non-enzymatic ketone test strip. In this modification, a separate glucose reagent pad and separate ketone pad are mounted on the same support. Both pads are covered with a blood separation coating. Two drops of blood, one for each separate reagent pad, are applied to the device. The user manually times the reaction by allowing the blood to soak in for one minute, and then manually wipes or washes off the excess blood from the outer layer of the pad.
As taught, the device of U.S. Pat. No. 4,397,956 measures whole blood acetoacetate using the sodium nitroprusside reaction, rather than the preferred enzymatic beta-hydroxybutyrate specific reaction. Thus the test reagent of U.S. Pat. No. 4,397,956 would be expected to suffer from the previously mentioned beta-hydroxybutyrate insensitivity clinical deficiencies of this type of reaction chemistry. This clinical deficiency, on top of other test deficiencies such as the requirement for multiple blood sample application steps, and extensive user intervention (timing, washing) teaches against the need for a competitive and automated dual glucose/beta-hydroxybutyrate whole blood test.
Prior art for single analyte glucose electrochemical sensors can be found a variety of patents, including many assigned to Genetics International, Medisense, E. Heller, & Company, Therasense, Selfcare, Boehringer Mannheim, and others. These include U.S. Pat. Nos. 4,545,382; 4,711,245; 4,758,323; 5,262,035; 5,262,305; 5,264,105; 5,286,362; 5,312,590; 5,320,725; 5,509,410; 5,628,890; 5,682,884; 5,708,247; 5,727,548; 5,820,551; 5,951,836; 6,134,461 and 6,143,164;
Prior art for single analyte hydroxybutyrate electrochemical sensors was published by Batchelor, et. al, “Ampherometric assay for the ketone body 3-hydroxybutyrate” Analytica Chimica Acta 221 (1989), 289-294.
U.S. Pat. No. 4,225,410 discloses an integrated array of electrochemical sensors where each sensor is a complete self-contained electrically isolated electrochemical cell, mounted on a solid support that contains a plurality of such cells. As is the case for previous art covering multiple colorimetric reagent pads on a single solid phase support, placing multiple electrically isolated electrochemical cells on a single solid phase support is also unsuitable for small rapid, low cost, analysis of 1-10 ul volume whole blood samples. Due to the surface tension characteristics of blood, separation of a single 1-10 ul droplet of whole blood into multiple electrically isolated droplets must overcome surface tension effects, and thus is energetically unfeasible without the intervention of energy added by some extra mechanisms. Although such mechanisms are known in the art (e.g. U.S. Pat. No. 6,090,251, etc.), the extreme manufacturing cost sensitivity of practical blood glucose tests should be recognized. Any commercially practical dual-purpose glucose-beta-hydroxybutyrate or other relevant second analyte electrochemical sensor must be price competitive with mass marketed single purpose glucose sensors, which can typically be produced at costs of about 10-20 cents per sensor. This brutal economic constraint on manufacturing costs eliminates all but the simplest combined designs from consideration. At the present state-of-the art, it appears unlikely that means will be found to mass produce, for a total cost of 10 to 20 cents per unit, a fully functional combined purpose electrode-containing-reagent, that also contains extra mechanisms to reliably and almost instantly separate a microliter sized drop of blood into two or more electrically isolated droplets.
WO 99/58709 discloses dry reagent test devices with two electrochemical sensors, but fails to teach mixed electrochemical/optical devices or pure optical devices. No commercial product based on WO 99/58709 has been announced to date.
Prior art for electrically triggered optical test reagents includes U.S. Pat. Nos. 5,344,754 and 5,554,531.
Prior art for fiber optical biochemical sensors includes U.S. Pat. No. 4,682,895, which teaches fiber optical probes with sharp, 180-degree bends at the sensor tip. Other prior art includes U.S. Pat. No. 4,548,907, which teaches bifurcated optical probes for use with pH dependent fluorophores, and U.S. Pat. No. 4,910,402 which teaches a dual fiber optic sensor for drop-sized samples.
Prior art for turbidity sensors includes U.S. Pat. Nos. 3,586,862, 3,665,301, 3,714,444, 4,055,768, 4,211,530, 4,841,157, 4,910,402, 5,350,992 and 5,940,148.
SUMMARY OF THE INVENTION
The two major detection methods employed in modern dry reagent blood glucose tests are calorimetric (best exemplified by the LifeScan “One-Touch” and “SureStep” systems), and electrochemical (best exemplified by the Medisense “Precision” family of systems). All work with extremely small sample sizes, typically under 10 ul, and all are “automatic” in the sense that after the addition of a single drop of blood, all further analysis and data reporting is done automatically by the meter. These systems set the standard for performance that a successful combined glucose/beta-hydroxybutyrate; a combined glucose/chylomicrons or glucose/triglycerides, or other combined glucose/other-analyte reagent must match or exceed.
In this disclosure, reagents, systems and methods to add additional whole-blood beta-hydroxybutyrate detection and reporting means, additional chylomicron or triglyceride detection and reporting means, or other additional analyte detection and reporting means to novel and state-of-the-art blood glucose reagents are disclosed. Such systems and methods disclosed herein are designed to enable the combined test to have performance characteristics similar to modern dedicated single-purpose blood glucose reagents.
According to this invention, the main principle that applies throughout is that both sensors in the combined reagent device should be held so close together that both can be simultaneously rehydrated (or hydrated) and activated using a single, unseparated, whole blood drop. Because the two sensors are so close together, however, the system must also be designed to minimize “cross-talk” between the two different neighboring sensors.
Enzymatic detection schemes: To briefly review, glucose, beta-hydroxybutyrate, and many other relevant second analytes can be detected using a variety of different enzymatic schemes.
Glucose reacts with the enzyme glucose oxidase. In an electrochemical system, the electrons will then transfer to an electron transfer mediator molecule, such as ferrocine, and then enter the reagent's electrode. In an optical system, glucose oxidase will produce hydrogen peroxide. This in turn will react with a second enzyme, peroxidase, and an indicator dye molecule, such as a benzidine dye.
Alternatively, Glucose may react with a dehydrogenase enzyme, such as hexokinase/glucose-6-phosphate dehydrogenase. This will convert NAD to NADH. In an electrochemical test, the NADH in turn will undergo electron exchange with an electron transfer mediator molecule, such as 4-methyl-o-quinone. This in turn transfers electrons to the reagent's electrode. In an optical system, the NADH will in turn react with the enzyme diaphorase and an optical indicator molecule such as a tetrazolium dye like INT (2-(4-iodophenyl)-3-(4-nitrophenyl)-5-phenyl tetrazolium chloride).
Similarly, beta-hydroxybutyrate reacts with the enzyme beta-hydroxybutyrate dehydrogenase (E.C. 1.1.1.30). This will then convert NAD to NADH. In an electrochemical test, the NADH in turn will undergo electron exchange with an electron transfer mediator molecule, such as 4-methyl-o-quinone. This in turn transfers electrons to the reagent's electrode. In an optical system, the NADH will in turn react with the enzyme diaphorase and an optical indicator molecule such as a tetrazolium dye like INT (2-(4-iodophenyl)-3-(4-nitrophenyl)-5-phenyl tetrazolium chloride).
Turbidity detection schemes: As discussed by Tazuma et. al. (“A quantitative assessment of serum chylomicron by light scattering intensity: Application to the intestinal fat absorption test”, Journal of Gastroenterology and Hepatology, Volume 12(11), November 1997, pp 713-718), and by Thorp et al (Thorp J M, Horsfall G B, Stone M C. A new red-sensitive micronephelometer. Med. Biol. Eng. Comput. 1967; 5: 51-6); turbidity measurements obtained by light scattering from small plasma or serum samples (micronephelometric methods) correlate well with chylomicron triglyceride levels obtained from more standard clinical assays.
A more detailed review of the various enzymatic methods may be found in: “Introduction to Bioanalytical Sensors” by A. Cunningham, published by John Wiley & Sons, 1998, the contents of which are incorporated herein by reference. A more detailed review of various turbidity (nephelometric) methods may be found in U.S. Pat. No. 5,940,178.
Techniques to correct for cross talk effects for two neighboring electrochemical tests were previously discussed in parent application Ser. No. 10/264,206, paragraphs 42-47, the contents of which are incorporated herein by reference.
Whole blood turbidity measurements pose challenges that have not been completely addressed by prior art. The pioneering work of Tazuma and Thorp, previously discussed, was performed with plasma or serum samples. Plasma and sera require that whole blood be centrifuged, subjected to membrane filtration, or subjected to a clotting process, and thus this type of sample is not suitable for incorporating into extremely rapid, extremely small volume, modern commercial blood glucose tests. Any attempt to measure the turbidity caused by chylomicrons and other lipoproteins in whole blood samples must contend with the very high interfering level of light absorption and light scattering caused by the large concentration of red cells. Red cell hemoglobin intensely absorbs visible light, making long optical pathways, required to generate an optical scattering signal, infeasible. Red cells also scatter light. As a result, optical interference caused by red cells tends to dominate the smaller amount of light scattering (turbidity) caused by chylomicrons, which is why previous workers chose to remove red cells and perform their light scattering studies with red-cell-free plasma or serum. To detect chylomicrons in whole blood using light scattering techniques, the analytical system must be designed to compensate for this very large red-cell optical background signal.
A number of techniques can be done to reduce the magnitude of the interfering red-cell optical signal to a manageable level. A first important step is to utilize the fact that red-cell hemoglobin has very low absorbance in the far-red and near infrared spectral region (Zijlstra, et. al. Clin. Chem. 37/9, 1633-1638, 1991), which enables much longer optical paths at these wavelengths (approximately 650 to 1400+ nm, where nm is the standard abbreviation for nanometers). A second important step is to utilize the fact that since red cells are much bigger than chylomicrons, red cells will tend to scatter light at different angles, and this difference in scattering efficiency as a function of angle can be used to separate the chylomicron and lipoprotein light-scattering signal from the background red-cell scattering signal.
The present invention utilizes these two facts: 1) longer optical paths through whole blood are possible at far-red and near infrared wavelengths, and 2) particles of different size scatter light at different angles; to construct extremely simple dual whole-blood glucose/lipoprotein test strips.
The optical equations used to calculate light scattering are well understood. One equation that is often used for light scattering calculations of this sort is Mie theory which describes the light scattering of particles of this approximate size (Johnsen and Widder, “ The Physical Basis of Transparency in Biological Tissue: Ultrastructure and the Minimization of Light Scattering ” J. Theor. Biol. (1999) 199, 181-198, and Ruf and Gould “ Size distributions of chylomicrons from human lymph from dynamic light scattering measurements ” Eur. Biophys J. (1998) 28: 1-11).
Mie theory calculating programs, such as “Scatlab” (Bazhan V., Scatlab 1.2 software, www.scatlab.com) allow researchers to calculate the amount of scattering, as a function of scattering angle, which is caused by various particle types under various conditions. Here the relevant parameters are the wavelengths of light (here near-infrared wavelengths of approximately 700 and 1000 nm can be used), average chylomicron diameter (approximately 0.1 microns, with a range between 0.05 and 0.3 microns), chylomicron index of refraction (about 1.46), average red cell diameter (approximately 5 microns, with a range between about 2 to 8 microns), average red cell index of refraction (about 1.4), and the index of refraction of the surrounding plasma media (about 1.34). Using these parameters, the Scatlab Mie calculator generates the following table of normalized scattering intensity at various angles, wavelengths, and particle types:
TABLE I
Relative (normalized) scattering intensity versus particle size, angle, and
wavelength.
700 nm
1000 nm
Small C
Medium C
RBC
Small C
Medium C
RBC
Scattering angle
.1 micron
.2 micron
5 micron
.1 micron
.2 micron
5 micron
0° (no scattering)
100%
100%
100%
100%
100%
100%
20° to 0° ratio
89.54%
72.62%
0.03%
92.54%
83.34%
0.08%
30° to 0° ratio
78.81%
49.70%
0.02%
84.56%
67.36%
0.03%
45° to 0° ratio
59.87%
21.69%
0.01%
69.52%
42.44%
0.02%
90° to 0° ratio
27.16%
2.96%
0.01%
39.82%
12.40%
0.02%
160° to 0° ratio
22.03%
3.17%
0.01%
59.24%
2.27%
0.02%
180° to 0° ratio
21.68%
3.05%
0.01%
61.76%
2.17%
0.02%
In Table I, the scattering caused by two populations of chylomicron particles (small 0.1 diameter particles and medium sized 0.2 micron diameter particles), and the scattering caused by a representative red blood cell (5 micron diameter) population is shown at 0° (no scattering), 20, 30, 45, 90, 160 and 180° angles from the incident light. These calculations are done at two near-infrared wavelengths (700 nm and 1000 nm), which are not absorbed by red cell hemoglobin, and thus penetrate for a substantial distance through whole blood.
The table I scattering data shows that back-scattering turbidity detectors, which measure scattering angles of approximately 180°, are particularly useful for this application. The chylomicron-sized particles generate a comparatively high degree of 180° backscattering, while red blood cells have almost no 180° backscattering. Thus the 180° backscattering signal is almost totally caused by chylomicrons, which simplifies data analysis. An additional advantage of the backscattering approach is that it is highly compatible with simple test strip designs. The small sample size and limited space available in a typical electrochemical blood-glucose test-strip, while giving relatively little additional “real estate” for other sensors, does provide enough room for optical backscattering detectors. In this configuration, both the light source and the light scattering detector (which may be as small as a light emitting optical fiber and a light receiving optical fiber) can be mounted on the same support base. This support base can also be used to hold the test-strip sensor electrodes as well.
Table I also shows that side-scattering and low-angle scattering turbidity detectors are also quite useful for whole blood turbidity measurements. The side-scattering geometry has its own set of advantages which tends to compensate for the somewhat more complex side-scattering test-strip design. In particular, note that the 0° angle (no scattering) parameter, shown in Table I, contains important information that can be used to compensate for (normalize) differences in illumination beam intensity. Side scattering designs also allow the sharp fall-off in the narrow angle red blood cell (RBC) scattering signal to be measured (note the Table I results showing that by 20°, the RBC scattering signal is almost zero). Additionally, the fairly large difference in scattering efficiency between the small 0.1 and medium 0.2-micron chylomicron particles at 700 nm and 1000 nm (Table I shows that at 45°, there is about a 2× difference between the 700 and 1000 nm results for 0.2 micron sized particles) can also be detected by use of a side-scattering geometry. This additional information can be used to more accurately estimate the true chylomicron concentration (since chylomicrons vary in size), as well as to better correct for distortion caused by red blood cell interference and other optical interference.
Thus for each type of test methodology, electrochemical or optical, the multiple test device must be designed to promote rapid access of a small (typically 20 ul or less) sample of whole blood to two different test sensors, and also must be designed to minimize cross-talk between the different test sensors or between the analyte and the red cell background. To the extent that some cross-talk still persists, the meter that reads the reagent may be designed in a way to facilitate the collection of sufficient data, and have sufficient onboard computing means, to do further analysis and mathematical deconvolution in order to accurately separate the two different signals, and distinguish them from background interferences.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a “sandwich” dry reagent electrochemical biosensor with glucose and beta-hydroxybutyrate electrodes on one surface, a chamber open on one end for receiving blood, and a reference electrode on a second surface.
FIG. 2 shows a “flat” electrochemical dry reagent biosensor with glucose and beta-hydroxybutyrate electrodes on one surface, and a reference electrode located above the surface.
FIG. 3 shows a combined optical analyte dry reagent test strip/meter system. The test strip contains a single blood separating membrane, with regions striped with glucose detection reagents on one track, and beta-hydroxybutyrate detection reagents on the other track.
FIG. 4 shows a dual mode optical-electrochemical sensor. This test strip consists of an electrochemical glucose sensor, and a fiber optic sensor, mounted so that both sensors can read the same drop of blood.
FIG. 5 shows a detail of the docking and optical interface between a dual mode optical-electrochemical sensor, and a meter. Here, the optical sensor consists of a single strand of optical fiber, capped with reagent.
FIG. 6 shows a “flat” dual mode electrochemical blood glucose test strip and optical backscatter turbidity sensor, enabling simultaneous glucose and chylomicron determinations.
FIG. 7 shows an exploded view of a “sandwich” dual mode electrochemical blood glucose test strip and optical side-scatter turbidity sensor.
FIG. 8 shows a side view of the “sandwich” dual mode electrochemical blood glucose test strip and optical side-scatter turbidity sensor.
FIG. 9 shows a front view of the “sandwich” dual mode electrochemical blood glucose test strip and optical side-scatter turbidity sensor.
FIG. 10 shows a simple, two fiber-optic, dual mode electrochemical blood glucose test strip and optical backscatter turbidity sensor.
DETAILED DESCRIPTION OF THE INVENTION
Example 1
Combined “Sandwich” Electrochemical Glucose, B-Hydroxybutyrate Sensor with Glucose and Beta-Hydroxybutyrate Electrodes on a First Surface, and a Single Reference Electrode on a Second Surface
The “sandwich” design has certain advantages from the user interface perspective. This design acts to “sip” a small drop of blood into an interior cavity formed by the various layers. This helps to partially protect the sample from the outside environment during the reaction.
Although in examples 1 and 2 given here, glucose oxidase type electrodes are illustrated, it should be understood that the principles taught herein would apply to glucose dehydrogenase type electrodes and electrodes for other enzymatically detected analytes.
Methods:
A detailed discussion of the methods to construct suitable NADH and Hydrogen peroxide specific electrodes, as well as glucose and hydroxybutyrate specific electrodes, was previously discussed in parent application Ser. No. 10/264,206, paragraphs 54-61, the contents of which are incorporated herein by reference.
A diagram of a “sandwich” type prototype sensor is shown in FIG. 1 .
The prototype sensor may be produced by multiple screen-printing steps. Here the two working electrodes ( 102 and 103 ) are put on the same flat sheet of PVC ( 101 ) (or suitably prepared flat sheet of light-pipe material, if a secondary turbidity test is desired. Here “PVC” will be used to refer to any type of suitable flat support), and the reference electrode ( 107 ) printed on a second sheet of PVC ( 106 ), and then laminated on top of the fist PVC sheet with spacer ( 108 ) to form a sandwich structure with an opening to admit blood ( 109 ).
The PVC sheet ( 101 ) holding the glucose and beta-hydroxybutyrate working electrodes may be prepared as follows: In the first printing step, the traces ( 102 , 103 ) connecting the electrode areas to the external electrical connection means may be printed. In the second step, the NADH electrode ( 104 ) can be printed. In the third step, the H 2 O 2 electrode ( 105 ) is printed. In the fourth step, the NADH electrode ( 104 ) is overprinted with buffered saline solution containing 30 U/M1 D3-Hydroxybutyrate dehydrogenase, 10 mM NAD. In the fifth step, the H 2 O 2 electrode ( 105 ) is overprinted with a buffered saline solution containing 10,000 U/ml of aqueous Aspergillus Niger glucose oxidase. Each working electrode is 1 mm wide, and the two electrodes are separated by a gap of 1 mm. After each printing step, the electrodes should be dried in a convection oven at 65° C. for 30 minutes and then stored in a cool, dry, environment until the next printing step.
The PVC sheet holding the reference electrode may be produced in two screen-printing steps. In the first printing step, the traces connecting the electrode areas to the external electrical connection means are printed ( 107 ). In the second step, the reference electrode silver-silver chloride electrode ( 110 ) is made by screen printing Gwent product C61003D7 onto 20 mil thick PVC substrate using 156 mesh polyester screen. The electrodes are then dried in a convection oven at 65° C. for 30 minutes and stored in a cool dry environment until used. The reference electrode may be 3 mm wide.
The two PVC layers should then be laminated together with an additional 10 mil (0.254 mm) thick spacer layer to result in a sandwich electrode with 3 mm×3 mm sized electrode surface area, and an internal volume of about 2.2 ul. Note that the electrodes on surfaces 106 and 101 all face the interior of the cavity.
A detailed discussion of electrical sensing methods used to read the electrochemical test strips was previously discussed in parent application Ser. No. 10/264,206, paragraphs 67-71, the contents of which are incorporated herein by reference.
Other electrode chemistries and production methods are also possible. As an example of one alternative, electrodes can be produced in general accordance with the sol-gel graphite composite technology as taught by U.S. Pat. No. 6,231,920.
Methods to construct suitable graphite composite electrodes were previously discussed in parent application Ser. No. 10/264,206, paragraphs 73-78, the contents of which are incorporated herein by reference.
Coating electrodes with an inert hydrophilic, microporus layer: In order to help exclude as many interferents from the working area of the electrodes as possible, it is often advantageous to employ various microfiltration schemes to exclude red cells and other interferents. This may be done by a variety of means. The electrodes themselves may be designed to be microporous, as is taught by U.S. Pat. No. 6,231,920. Alternatively, or in combination, the electrode assembly may be covered with a microporous electrically inert material designed to admit sample while excluding as many interferents as possible. Such layers may be composed of previously synthesized filter materials, or built-up de-nouveaux on the test strip by means of self self-assembling chemical compositions, such as the mixed hydrophobic-hydrophilic particle techniques taught by U.S. Pat. Nos. 5,708,247 and 5,951,836.
Methods to construct suitable microporus layers were previously discussed in parent application Ser. No. 10/264,206, paragraphs 80-82, the contents of which are incorporated herein by reference.
As previously discussed, it is often advantageous to cap electrodes with such electrically inert microporus structures to reduce interference. Alternatively, such electrically inert microporous structures may be employed as “spacer” layers between stacked arrays of active electrodes, as is discussed in example 2.
Example 2
Multi-Layer Combined Glucose, Beta-Hydroxybutyrate Sensor
In an alternative embodiment, a porous spacer layer may be coated on top of the two sensor electrodes, and the reference electrode in turn coated on top of the spacer layer. Because the reference electrode is now elevated a significant distance above the primary support, an elevated stage with a secondary-conducting path may be added. Here a drop of blood is added directly to the primary support.
This “flat” reagent has its own unique set of advantages. Its more open design facilitates manufacturing. Additionally, some users may prefer applying sample to the more open reagent area.
This scheme is shown in FIG. 2 . In this scheme, conducting electrical paths ( 102 , 103 ) are laid down on support ( 101 ) followed by the glucose and beta-hyroxybutyrate electrodes ( 202 , 203 ). Usually this is done by a screen-printing process. In subsequent screen-printing processes, porous spacer layer ( 204 ) is printed to help fluid flow. Glucose and beta-hydroxybutyrate reagents ( 205 , 207 ) are printed on top of the porous spacer layer and are absorbed into the layer. A second porous spacer layer ( 208 ) is then printed. An elevated stage ( 212 ) to carry the reference electrode signal to the meter may then be added, either by lamination or thick film printing. Finally, reference electrode ( 209 ) and reference electrode conductive paths ( 107 ) are printed. This reference electrode may contain one or more open regions ( 210 ) to allow the applied sample to flow to the lower layers. In some embodiments, it may be advantageous to apply a final porous layer on top of reference electrode ( 209 ) to stabilize the electrode stack, and reduce imprecision due to hematocrit effects or other interferents.
In operation, a drop of blood is placed on top of reference electrode ( 209 ). The blood flows through electrode gap ( 210 ) into porous spreading layer ( 208 ). The blood then flows into porous electrodes ( 207 ) and ( 205 ). Electrical signals from glucose and beta-hydroxybutyrate production ( 202 , 203 ) are conducted to the meter through electrical paths ( 102 , 103 ). The reference electrode signal is conducted to the meter though elevated electrical path ( 107 ) on an optional different surface ( 212 ) elevated above first surface ( 101 ).
Although electrochemical based glucose tests are rapidly becoming the preferred modality for this type of reagent, it is also possible to create simple, easy to use, one blood drop activated optical glucose+beta-hydroxybutyrate (or other relevant second analyte) reagents as well. This is shown in example 3.
Example 3
Optical Combined Glucose/Beta-Hydroxybutyrate (or Other Relevant Second Analyte) Test Strip
In this example, a blood separating membrane, such as the membranes produced using the highly asymmetric membrane technology of the Filterite division of Pall corporation (“asymmetric polysulfone membranes”, see U.S. Pat. Nos. 4,774,192 and 5,968,836) may be used to conduct the basic reaction. Typically filter membranes rated between 0.8 and 0.2 microns are preferred for this purpose. Asymmetric polysulfone membranes, used in this example, have a variable porosity structure with a large pore side on one side of the membrane, where sample is typically applied, and a small pore side, where the reaction results are typically observed.
Red cells in the blood sample applied to the large pore side migrate only partially into the membrane matrix, where they become trapped. By contrast, the plasma portion of the blood is free to move all the way to the small pore side. The membrane has sufficient optical opacity that if whole blood is applied to the large pore side of the membrane, only clear plasma is observed on the small pore side. Thus the color and reaction obscuring properties of the red cell hemoglobin are removed from the reaction. By embedding the appropriate reaction chemistry into the membrane, various types of chemical analytes can be observed, in particular, glucose and beta-hydroxybutyrate.
The small pore side of the membrane can be left open to the air. Alternatively, the small pore side may be covered with a transparent layer. Such transparent coverings may be desirable to improve reaction uniformity, resistance to environmental variables, and to reduce the chance of plasma from the sample contaminating the underlying meter. Such transparent membranes can reduce oxygen flow to the reaction however. Although this is not a problem for non-oxygen dependent enzymatic reactions, such as the beta-hydroxybutyrate reaction, it can be a problem if the commonly used glucose oxidase reaction for detecting glucose is used. Such glucose detection reactions are oxygen dependent, and thus might function sub optimally if the reaction matrix has a transparent layer that does not conduct oxygen well.
In this situation, use of the hexokinase glucose (glucose dehydrogenase) detection chemistry may be favored, since such reactions are not oxygen dependent. Additionally, such reactions use a number of the same reaction intermediates (NAD-NADH) and enzymatic reaction facilitators (diaphorase) etc., as the beta-hydroxybutyrate reaction. This may simplify test reagent construction, since the base membrane may be coated with reaction chemistry common to both enzymatic reactions, and the chemistry specific to each particular reaction may be then applied or streaked on in subsequent steps.
In order to work with a single 1-10 ul sized drop of blood, both the glucose and the second analyte (such as beta-hydroxybutyrate) reaction zones should be situated close to each other. As an example, membrane in the reaction zone may be coated with the glucose specific chemistry on one half, and the beta-hydroxybutyrate chemistry on the other half. The two half sides may be separated by a gap, or by a semi-permeable “speed bump” zone. Alternatively, the membrane may be intermittently sealed in a dotted line fashion between the two sides, so that cross-diffusion between sides is reduced, yet the two areas still remain in fluid communication.
Since beta-hydroxybutyrate or other second analyte detecting reagents will tend to be expensive, in an alternative configuration, it may be preferable to spot a smaller “dot” or “stripe” of the second analyte reagent onto a membrane otherwise nearly 100% saturated with the glucose reagent. In this case, the second analyte chemistry should be selected as to be resistant to the distortions caused by the large amount of neighboring glucose detection chemistry. This may be accomplished by a variety of means, such as incorporating a hydrogen peroxide absorbing or inactivating chemistry in the second analyte reagent. In this case, the user will either be expected to judge the color of the dot or stripe by eye, or alternatively the meter may contain means, such as a linear photodetector array, etc., to image the spot or stripe, and calculate and report a separate measurement.
In yet another alternative embodiment, the two regents may be applied to the surface of neighboring optical fibers or optically conductive pathways (such as an optical “light pipe”), one reagent per optical light-pipe. A holder that exposes both fibers to the same drop of blood may hold these optical light pipes together. In this case, the meter will contain means to independently interrogate the two optical light pipes, and report separate measurements.
In order to help visually distinguish this combined analyte test strip from the more commonly used single analyte test strip, it may be advantageous to include a tracking dye with either the glucose specific or second analyte specific second coating. A user could then use the colored stripe to help visually distinguish the combined test strip from the single analyte test strip.
In order that the tracking dye not interfere with subsequent colorimetric analysis of the reaction (either visual or photometric), it would be further advantageous if the dye rapidly undergo a transition from colored to uncolored (or alternate color) soon after sample application. Any dye that does not otherwise interfere with the reaction chemistry may be used here. As one example, the pH tracking dyes methyl red or phenol red may be applied to the surface of the membrane in a thin layer at pH that is mildly acidic relative to the rest of the reagent membrane. This thin layer is rapidly air dried immediately after application to keep the tracking dye distinct from the rest of the reagent in the membrane.
Under mildly acidic conditions, suitable pH tracking dyes absorb intensely around 520-550 nm and appear yellow. Upon application of sample, the dyes will mix with the more alkaline conditions in the applied sample and dried buffer from the rest of the membrane reagent, transition to a less acidic environment, and change their spectral properties. In particular, the dyes intense absorbance at 520-550 nm will stop (and thus the observed reflectance in the spectral region between 500-580 nm will increase), and instead the dyes will absorb at around 435 nm, and appear red. One advantage of this spectral response is that many indicator dyes useful for glucose and beta-hydroxybutyrate reactions have absorbance maximums that extend well into the 600 nm region, and thus there will be no additional cross-talk with the less acidic form of the pH indicator dyes. Many other dye reactions are possible and suitable, however.
A further advantage of such a tracking dye that undergoes a colored to clear transition upon hydration is that it can be used to help insure correct registration and tracking in an automated meter reader system. A frequent problem with such tests is that if a test strip reagent is not fully inserted (for example is only inserted so that half of the reaction zone is visible to the photo-optical reader), and then triggered by a optical reflectance drop (such as taught by U.S. Pat. Nos. 5,049,487; 5,843,692 and 6,268,162), then there is a significant possibility that the reaction would proceed with the meter reading only part of the colorimetric indicator. This could result in a potentially serious measurement error.
A meter designed to read a visually based combined functional glucose-second analyte test strip will normally have two photodetector systems, one designed to read the glucose portion, and the other designed to read the second analyte portion.
The asymmetric polysulfone membranes used in the examples here differ from the nylon membranes previously employed in the reflectance drop triggering methods of U.S. Pat. Nos. 5,049,487 and 5,843,692. Typically the color drop upon the placement of blood on an asymmetric polysuflone membrane is considerably less than the color drop upon the placement of blood on a nylon membrane. This is because the red-cell lytic nature of nylon membranes causes hemoglobin to rapidly transfer to the observation side of the nylon membrane. By contrast, non red cell lytic membranes, such as asymmetric polysuflone membranes, conduct relatively small amounts of hemoglobin to the observation side of the membrane. Thus use of reflectance drop techniques to detect sample application is relatively problematic when using reagents employing non-red cell lytic membranes are used.
By contrast, use of the color change of a tracking dye, induced by sample induced membrane hydration, has a number of advantages for test triggering purposes. Here, the test reagent is optimally designed so that the test strip must be fully inserted in order to bring the tracking dye portion of the membrane into full view. The meter can then be programmed to repeatedly interrogate the reflectance of the tracking dye portion of the membrane. Upon addition of sample, the tracking dye will then transition from a colored state to a non-colored state (or alternate color state), and the increase in reflectance at one or more wavelengths can then be used to trigger the start of the reaction. If the test strip is not fully inserted, or if the wrong type of test strip is used, the device will not trigger. This provides extra protection against user errors.
Modern blood glucose meters are extremely fast, and to be competitive, a dual-purpose glucose-second analyte reagent/meter system must also be as fast as possible. Here the reaction chemistry imposes some constraints, however. A sample with a high level of glucose or beta-hydroxybutyrate will typically take longer to complete than a reaction with a low level of these analytes. By necessity, an instrumented test that waits a fixed amount of time after reaction initiation in order to be sure to properly measure a sample containing a higher level of analytes will proceed with sub-optimal time efficiency with samples containing a lower level of analytes. In order to be as fast as possible, therefore, it is further advantageous to photometrically sample the reagent multiple times during the reaction, make real-time assessments as to if the reaction is heading to completion, and terminate the variable length test as soon as feasible.
FIG. 3 shows an exemplary combined optical glucose, second analyte sensor. A plastic support ( 301 ) with a center aperture carries membrane ( 302 ), which may be covered by optional transparent layer ( 303 ). In this example, both the glucose and the exemplary beta-hydroxybutyrate reaction use dehydrogenase enzymes.
Label 320 shows a view from the top of plastic support ( 301 ) looking down on membrane ( 302 ) from above. Center aperture ( 321 ) can be seen. Membrane ( 302 ) has typically been first coated throughout with a reaction solution typically containing a buffer, reaction cofactors such as NAD and diaphorase enzyme, and typically one or more polymers and non-glucose sugars to stabilize the reaction components, and helps modulate fluid flow. Membrane ( 302 ) will also contain two tracks. These tracks are usually produced by a second overcoating step using a thin layer of overcoat reagent solution followed by rapid drying.
One track ( 322 ) will contain the complementary enzyme for one of the two test reactions, such as hexokinase glucose, an indicator dye, and other reaction cofactors. A second track ( 323 ) will contain the complementary enzyme for the other test reaction, such as beta-hydroxybutyrate dehydrogenase and other reaction cofactors. A second reagent indicator dye, (ideally with a different spectral response from the first indicator dye to minimize cross talk), will also be included. The second reagent track will usually be separated by gap ( 324 ) from the first reagent track.
Often, it may also be advantageous to include a moisture sensitive tracking dye (shown as the crosshatched area in ( 323 )) that changes color from dark to light upon the addition of sample, into one or more of the two reagent tracks.
In operation, 1-10 ul (more generally 0-20 ul) of whole blood ( 304 ) is applied to the sample-receiving (open pore in the case of asymmetric polysulfone) surface of membrane ( 302 ). Red cells and plasma are separated and plasma flows through to the optical reading side, which may be covered by optional transparent membrane ( 303 ). The reaction zones ( 322 ) and ( 323 ) become hydrated with sample.
While this is going on, the underside of the test strip is being observed by a microprocessor controlled optical stage underneath the membrane ( 305 - 312 ). In operation, the optical stage periodically polls the state of tracking dye-coated membrane ( 323 ). This is done by a light source ( 308 ), controlled by microprocessor ( 313 ). This light illuminates the underside of the test strip ( 302 , 303 ) and is detected by a microprocessor-controlled photodetector ( 310 ).
Typically light sources ( 305 ) and ( 308 ) will be provided by light emitting diodes (LEDs), and have defined spectral characteristics. In particular, light source ( 308 ) will optimally have spectral characteristics optimized to be sensitive to the color transition of the tracking dye, and also sensitive to the color transition of the indicator dye. If one LED does not have the required wavelength spectral properties for both purposes, two LEDs (or other light sources) with different spectral properties may be used in ( 308 ).
Upon sample addition, tracking dye ( 323 ) alters its spectral state and the increase in reflectance on at least one wavelength is detected by photodetector ( 310 ). This initiates test timing. Both reaction zone areas ( 322 ) and ( 323 ) are observed periodically by light source ( 305 ) and photodetector ( 307 ) (for zone ( 322 )) and by light source ( 308 ) and photodetector ( 310 ) (for zone ( 323 )). Note that depending upon the optical geometry, the same photodetector may be used for both ( 307 ) and ( 310 ).
The microprocessor ( 313 ) monitors the kinetics of both reactions. When it accumulates enough data points to either determine reaction rate, or extrapolate reaction endpoint levels, microprocessor ( 313 ) stops accumulating further data, calculates the final answer, and typically will display both answers on display ( 314 ).
In an alternative embodiment, the device of FIG. 3 can be configured to be a dual glucose-blood turbidity sensor. In this alternative embodiment, half of the membrane (portion 322 ) is omitted, and the transparent support 303 is present. As a result, the 322 portion of window 321 allows a direct view of the blood sample, while membrane 323 allows an analyte, such as glucose, to be determined by the enzymatic calorimetric techniques discussed previously. In this scheme, light-emitting diode 305 is configured to emit near-infrared light (i.e. light with a wavelength greater than about 650 nm), and photodiode 307 is configured as a backscattering turbidity detector. This backscattering signal can then be converted to a triglyceride concentration (using a conversion equation such as equation 1), chylomicron concentration, or other marker of relative lipemia levels.
Example 4
Combined Electrochemical—Optical Sensor
In this example, a hybrid detector element is formed containing one detection element based upon electrochemical technology, and a second detection element based upon optical technology.
Here, the electrochemical element may be a conventional electrochemical detector element, such the electrochemical glucose sensors discussed previously. The optical element may be a membrane based optical sensor, such as the optical membrane beta-hydroxybutyrate sensors discussed previously, or an alternate type of optical sensor.
One advantage of electrochemical sensors, however, is that the sensor element only needs to be connected to a meter by an electrical contact. As a result, electrochemical sensor-meter systems can be designed in which the electrochemical detector protrudes a significant distance away from the main body of the meter. This improves the user interface, because a drop of blood can be more easily applied to the protruding sensor. Additionally, it is often easier to insert or remove sensors if they stick out from the main meter body.
By contrast, membrane based optical sensors typically need to be held closely to the optical portion of a meter. This makes sample application more difficult, as applied blood thus has a higher chance of smearing onto non-sensing regions of the meter body, creating an undesired mess.
To avoid these ergonomic issues, it may often be advantageous to use an optical conductive pathway, such as a molded optical wave guide, optical fiber, “light-pipe” or the like to transmit the optical signal from the second optical sensor to a detection device. The optical wave-guide carries the optic signal along the same pathway used to conduct the electrical signals. Because the optical reagents need be applied only to the tip of the optical wave-guide probe, only extremely small amounts of reagent and blood are needed for the reaction. As a result, an optical sensor may be added to an electrochemical sensor with only minimal perturbation to the design of the electrochemical sensor.
A diagram showing this combined electrochemical optical sensor is shown in FIG. 4 . Here, the support substrate ( 101 ) contains electrodes ( 102 , 103 ) making contact with conventional glucose electrochemical reagents ( 404 , 405 ). This, in turn, is separated by a spacer layer ( 108 ) from second support substrate ( 106 ). In practice, first support substrate ( 101 ), spacer ( 108 ), and second support substrate ( 106 ) are combined to form a single unit, containing a chamber ( 109 ), which is used to receive the blood sample.
The unit additionally contains at least one optical wave-guide element ( 408 ) placed between support substrate ( 101 ) and ( 106 ). This optical wave-guide may be tipped with a colorimetric, fluorescent, or luminescent reagent ( 409 ), such that the analyte in the blood admitted to reaction chamber ( 109 ) produces a detectible optical signal, which is transmitted to an optical detection apparatus or meter by way of optical wave guide ( 408 ). Alternatively, when a turbidimetric or other measurement not requiring a separate reagent is used, the optical wave guide (or light pipe) need not be tipped with any reagent.
The configuration of optical wave-guide or light pipe ( 408 ) may be optimized for the specifics of the meter design and reaction chemistry. In some embodiments, it may be desirable to utilize an asymmetric design in which the meter side of the optical wave-guide is larger than the sample side of the optical wave-guide. This will facilitate optical coupling between the meter's optical excitation source and detector, and the wave-guide. At the same time, the sample side of the wave-guide can be kept extremely small, which minimizes the amounts of reagents and blood needed for the test.
Reagents, if needed, may be applied to the sensor end of the optical wave-guide with appropriate particulate or polymeric agents so as to create a relatively tough, but fluid permeable, cap on the tip of the wave-guide. Reaction chemistry indicator dyes and detection wavelengths may be chosen to give optimal signal-to-noise ratios with whole-blood samples. This favors the use of indicator dyes and detection wavelengths operating in the red and infrared end of the spectrum (greater than 650 nm), where interference from the hemoglobin present in whole blood is relatively minimal.
For colorimetric detection chemistries, it may often be advantageous to use multiple wavelength detection means employing both an indicator dye detection wavelength, and a reference wavelength where the indicator dye does not absorb as strongly. In this way, distortion of the calorimetric signal due to varying levels of hemoglobin or other interfereants in the sample may be minimized.
The configuration of the optical wave-guide may also be optimized for the problem at hand. As an example, in some situations, it may be advantageous to employ a dual chamber optical wave-guide with separate or partially separate optical conduits for the excitation signal and return signal. In other cases, a plurality of optical wave-guides may be advantageous.
For configurations employing reagents generating an optical signal, and single-fiber optical wave guides (fiber optics), use of fluorescent indicator dyes has certain advantages. The excitation wavelength, and the return fluorescent wavelength from the indicator dye, may travel through the same optical fiber with minimal confusion or cross-talk. Due to the extreme cost sensitivity of high volume mass-market glucose test strips, simple designs such as this are helpful. Simple reagent designs, which use minimal amounts of optical materials or reagents, have inherently lower production costs.
In the single fiber configuration, the reagent test-strip itself is kept extremely simple to reduce costs. Here, the single optical fiber is plugged into the optical unit of a meter, and any additional optical processing, beam splitting, and the like is performed by the meter's optical sensor unit. Ideally, to reduce costs to a minimum, the meter's optical sensor device is a miniaturized integrated optical chip, such as a MEMS optical chip.
In operation, sample is applied to reaction chamber ( 109 ). This sample interacts with the electrochemical sensor, producing a change in the electrical characteristics of the electrodes, such as an amperometric, potentiometric, conductometric, impedance, or other electrically detectible change, that signals the start of the test.
The meter will contain both electrical means to monitor the electrochemical reaction, and optical means to monitor the optical reaction. The meter monitors the reaction progress of the electrochemical reaction through electrical contact with electrodes ( 102 , 103 ). The meter uses the same electrical signal used to trigger the start of the electrochemical reaction to begin monitoring the optical reaction through optical contact with optical wave guide ( 408 ).
Usually, but not always, the electrochemical reaction will proceed faster than the optical reaction. The meter may be programmed to immediately report the electrochemical reaction, and additionally may be programmed to either always display the optical reaction, or alternatively only display the optical reaction if the results of the electrochemical reaction suggest that the optical reaction results may be medically relevant.
As an example, the meter may be programmed to immediately report glucose, and not indicate that a second beta-hydroxybutyrate reaction is proceeding, unless the glucose results fall into a high range where ketoacidosis is a genuine possibility. However if the glucose level falls into a range where ketoacidosis is a potential concern, the meter may display an alternative message such as “Wait-checking ketones” while the ketone test automatically continues. In this way, the test may proceed with optimum speed most of the time, while still providing a valuable emergency ketoacidosis warning.
Alternatively, when a dual glucose/lipoprotein (triglycerides, chylomicrons) test is desired, and the lipoproteins are detected by light scattering (turbidimetric) methods that are also very fast, the meter may display the glucose measurement as a number and the turbidimetric chylomicron or lipoprotein light scattering measurement as a bar graph of varying height. The human factors advantage of this mixed numeric-graphic display is that the less critical chylomicron reading will not distract the user from the more immediately urgent numeric blood glucose reading. This mixed display still allows both results to be read at a glance, however. Many other display schemes, such as large and small numbers, different colors, etc. are also possible.
Note that although FIG. 4 shows a fiber optical wave guide operating in conjunction with an electrochemical sensor where both electrodes are on the same solid support, it should be obvious that these concepts will apply equally well to other electrode configurations as well. As an example, each electrode could be mounted on a different support surface, such as surfaces ( 101 ) and ( 106 ). Alternatively, electrode configurations as shown in FIG. 2 may be used.
FIG. 5 shows a close up of the interface between a test strip ( 501 ) containing an opening to admit a sample ( 109 ), a single fiber optic sensor ( 408 ); docking to meter ( 504 ). This test strip may additionally contain electrochemical sensor electrodes (not shown) that also make contact with meter ( 504 ).
In this scheme, optical fiber ( 408 ) docks with an optical adapter element ( 505 ), which further may split the optical signal between a wavelength emitter element ( 506 ) and a detector element ( 507 ). Ideally, to reduce manufacturing costs, two or more of these detector elements and or adapter unit ( 505 ) are integrated onto a single custom optical chip ( 508 ). The information from the optical detector, and the electrochemical detectors, is then processed by a microprocessor, converted to a clinically useful set of values, and communicated to the user.
FIG. 6 shows a combination glucose-backscatter turbidity sensor based upon a flat electrode configuration. In FIG. 6 , the support material consists of two or three (three are shown) optically separate optical wave-guides or light-pipes 601 , 602 , and 603 (typically constructed of a transparent material, such as thin transparent plastic, with dielectric properties compatible with the electrochemical sensing portion of the test. Alternatively fiber optic fibers can be mounted on an appropriate support material) laminated together to form a flat base. To minimize interference from outside light and also to minimize cross-talk between light pipes, unless otherwise stated, the sides of each light pipe will usually be covered with an opaque (non-light conducting) material. However if the test-strip is to be mounted directly onto a meter optics block that performs the light scattering measurement, the support material may be transparent (not covered with an opaque material), and the light scattering may be observed directly.
One end of each light pipe is configured with a transparent optical connector 611 , 612 , and 613 so as to enable each light pipe to interact with an outside light source or optical detector on a meter (not shown). Each light pipe also has at least one additional optical window 621 , 622 , and 623 , typically formed by a gap in the opaque material covering the various respective light pipes. The three laminated light pipes 601 , 602 , 602 will typically form a continuous flat surface. The glucose sensing electrodes (for simplicity, only the conducing traces are drawn, and the actual electrode reagent pads are not shown) 102 and 103 will typically be formed on this flat surface. These electrodes are normally opaque, and in some configurations it may be desirable to lay out the electrodes in such a configuration as to optimize the openings in the opaque material surrounding the light pipe, consistent with the creation of optical windows 621 , 622 and 623 .
In use, a drop of blood (not shown) containing glucose, red cells, and light scattering lipoproteins is applied to the top surface of the sensor. Light from a meter optical source 632 enters the optical connector 612 on light pipe 602 . This light is conducted through the light pipe to light pipe optical window 622 . There the light beam 642 exits window 622 and will illuminate the lipoproteins 630 . Backscattered light 641 , 643 from lipoproteins 630 then enters light pipes 601 and 603 through optical windows 621 and 623 . This backscattered light is then conducted back through transparent optical connectors 611 and 613 , where re-emerges as backscattered light 651 and 653 . This can then be analyzed by the photodetectors on the meter.
The meter will also have electrodes capable of interfacing with test-strip electrodes 102 and 103 .
In addition to providing chylomicrons for the light scattering determination, the applied drop of blood also hydrates meter electrodes 102 and 103 . This signals the meter to perform a standard electrochemical blood glucose determination. At about the same time, the meter sends pulses of near-infrared light 632 through optical interface 612 . If there is a high level of lipoproteins present in the blood sample, the backscattered light signal 641 and 643 will be relatively high. This will be detected by meter photodetectors analyzing the light signal 651 and 653 reemerging from optical interfaces 611 and 613 . This signal can then be analyzed by the meter's microprocessor, and the user presented with a dual glucose-light scattering derived measurement. This light scattering measurement may be transformed by the meter's microprocessor, using a conversion equation such as equation 1, to a clinically relevant triglycerides, chylomicron level, or other measure of relative lipemic risk to guide the user in subsequent corrective action as needed.
Incoming light 632 may be composed of one or several wavelengths of light. If one wavelength is used, this will typically be a wavelength of about 700 nm or greater so as o have minimal absorption by the hemoglobin present in the sample's red blood cells. In some cases, however, it may be advantageous to use multiple wavelengths, such as 700 nm and either a shorter wavelength (useful for determining the amount of scatter caused by red cells in the sample) or a longer wavelength (useful for determining the relative size of the light scattering particles), or both. To reduce interference from outside light, the incoming light 632 will typically be switched on and off at high frequency intervals, and the meter's photodetector and analysis circuitry and program designed to use the light-off scattering signal to compensate for any stray background light signals that may interfere with the light-on scattering measurements.
Note that the locations of windows 621 and 623 do not need to form equivalent angles with light emitting from excitation window 622 . Rather, it may be desirable to arrange windows 621 and 623 so that one window is closer to excitation window 622 , and thus measures backscattered light closer to 180°, and the other window is further away from excitation window 622 , and thus measures backscattered light at alternate angles. The relative difference in intensity between the two signals can thus be used to estimate the relative size of the light scattering particles, and further discriminate between light scattered by the smaller lipoproteins and the light scattered by the larger red-cells.
Note that although FIG. 6 shows a three light-pipe configuration, in a more minimal implementation, only two light pipes (for example 601 and 602 ) will be needed to implement this type of sensor. These two light pipes could consist of two fiber optic fibers, one for excitation, and the other to collect the scattered light. In still other alternative configurations, the third light pipe may be configured to directly sample the light output from the excitation light pipe 602 , thus providing an excitation reference signal to the meter, which can be useful in normalizing or otherwise adjusting the light-scattering data for variations in the efficiency in light excitation energy.
FIG. 7 shows an exploded diagram of a “sandwich-type” combination glucose-side scattering turbidity sensor, in which blood samples migrate into a sensor cavity by capillary action. In FIG. 7 , the support material again consists of three optically separate optical waveguides or light-pipes 701 , 702 and 703 (typically constructed of a transparent material, such as thin transparent plastic, with dielectric properties compatible with the test's electrochemical sensors, or alternatively fiber optic fibers mounted on an appropriate support material) and unless otherwise stated may be coated with an opaque (non-light conducting) material to minimize interference from outside light, and to minimize cross-talk between light pipes. One end of each light pipe is configured with a transparent optical connector 711 , 712 and 713 so as to enable each light pipe to interact with an outside light source or optical detector (not shown). Each light pipe has either an additional optical window 722 or 723 or alternatively a central opening 109 through which light may traverse. The glucose sensing electrodes 102 and 103 will typically be formed on the top surface of light pipe 702 . These electrodes are normally opaque, and in some configurations it may be desirable to lay out the electrodes in such a configuration as to optimize the openings in the opaque material surrounding the light pipe, consistent with the creation of optical window 722 .
In use, a drop of blood (not shown) containing glucose, red cells, and light scattering lipoproteins (chylomicrons) is applied to opening 109 on the side of the sensor. Blood migrates into the central cavity 109 of the sensor by capillary action. Light from a meter optical source 732 enters the optical connector 712 on light pipe 702 . This light is conducted through the light pipe to light pipe optical window 722 . There the light beam 742 exits window 722 and will illuminate the lipoproteins 730 . Side scattered light 741 from lipoproteins 730 then enters light pipe 701 through optical windows 721 . This side-scattered light is then conducted back through transparent optical connector 711 , where it re-emerges as sides scattered light 751 . This can then be analyzed by the photodetectors on the meter and converted to a clinically relevant measurement by a conversion equation such as equation 1.
One advantage this side-scatter approach is that the non-scattered light 743 (or alternatively low-angle scattered light) can also be analyzed. This can then be used as a reference signal. If analysis of non-scattered light is desired, the placement of optical window 723 in light pipe 703 can be arranged directly over excitation light window 722 . Non-scattered light 743 then enters light pipe 703 , and is conducted to a photodetector on an outside meter (not shown) by way of optical connector 713 , where it emerges as non-scattered light 753 . Alternatively, if low-angle scattered light is desired, the optical window can be designed to be an annulus (ring) window 763 with the center part of the window 723 opaque to block non-scattered light, and the ring 763 transparent to allow low-angle scattered light to enter the device.
The meter will also have electrodes capable of interfacing with test-strip electrodes 102 and 103 .
In use, a drop of blood is placed on the test strip. This rehydrates meter electrodes 102 and 103 , and the meter performs a standard blood glucose determination. At the same time, the meter sends pulses of near-infrared light 732 through optical interface 712 . If there is a high level of lipoproteins present in the blood sample, the side-scattered light signal 741 will be relatively high. This will be detected by meter photodetectors analyzing the light signal 751 and reemerging from optical interfaces 711 . This signal can then be analyzed by the meter's microprocessor, and the user presented with a dual glucose-light scattering measurement. This light scattering measurement may be transformed by the meter's microprocessor to equivalent triglycerides, chylomicron level, or other measure of relative lipemic risk (such as postprandial lipemia analyte concentration) to guide the user in subsequent corrective action as needed.
Incoming light 732 may be composed of one or several wavelengths of light. If one wavelength is used, this will typically be a wavelength of about 700 nm or greater so as to have minimal absorption by the hemoglobin present in the sample's red blood cells. In some cases, however, it may be advantageous to use multiple wavelengths, such as 700 nm and either a shorter wavelength (useful for determining the amount of scatter caused by red cells in the sample) or a longer wavelength (useful for determining the relative size of the light scattering particles), or both. To reduce interference from outside light, the incoming light 732 will typically be switched on and off at high frequency intervals, and the meter's photodetector and analysis circuitry and program designed to use the light-off signal from the light scattering detection light-pipes to compensate for any stray background light signals that may interfere with the light-on scattering measurements. The difference in signal intensity between the side scattered light and the low-angle scattered light may also be used to determine the relative size of the light scattering particles.
FIG. 8 shows a side view of the sandwich style dual glucose-side scattering turbidity sensor previously shown in exploded form in FIG. 7 . In FIG. 8 , the three light pipes 701 , 702 and 703 are shown laminated together to form a single structure. The electrodes leading to the glucose sensors (here electrode 102 is shown, and 103 is hidden) are exposed to facilitate interface with socket on a meter capable of reading the glucose electrodes. The optical interfaces to the three light pipes, 711 , 712 and 713 are also exposed and are also designed to slide into a meter socket, usually a combination electrochemical and optical socket on a meter designed to perform simultaneous electrochemical and optical determinations. This meter socket will provide excitation light 732 into the excitation light pipe 702 by way of optical interface 712 . The meter socket will receive side-scattered light 751 from light pipe 701 by way of optical interface 751 . The meter may also receive low-angle scattered light or a non-scattered light reference signal 753 from light pipe 703 by way of optical interface 713 . This figure also shows a view of optical window 723 , here used to return a non-scattered light reference signal 753 .
FIG. 9 shows a front view of the dual glucose-side scattering turbidity sensor previously shown in exploded form in FIG. 7 , and in side view in FIG. 8 . In FIG. 9 , the three light pipes 701 , 702 , and 703 are again shown laminated together to form a single structure. The electrodes forming the blood glucose sensor 102 and 103 are also shown. The central cavity of the sensor, with the opening to admit blood, and the interior region where blood migrates by capillary action, is shown as 109 .
As before, a small drop of blood is applied to the test strip and this blood fills the central cavity 109 by capillary action. The fluid in the blood sample (not shown) activates the blood glucose sensors, and electrodes 102 , 103 electrically communicate the results. At the same time, lipoproteins (chylomicrons) in the blood sample (not shown) are illuminated by light 732 traveling through light pipe 702 , and exiting light pipe 702 through optical window 722 . Light side-scattered by the lipoproteins ( 741 ) enters light pipe 701 through optical window 721 . This is transmitted by light-pipe 701 and exits the light pipe by optical interface 711 as signal 751 , which is then read by a meter that connects to the optical interfaces and electrodes by a socket (not shown). Non-scattered light or low-angle scattered light 743 enters light pipe 703 . This in turn is transmitted by light pipe 703 and exits the light pipe by optical interface 713 as signal 753 . This is read by the same meter.
Alternate configurations are also possible. In an alternate embodiment of FIGS. 7-9 , the lower support 702 is transparent, the upper support 703 is made up of a black, non-reflective material, and the turbidity is measured by an optical system shining near-infrared light through support 702 , and measuring the backscattered turbidity through support 702 , using a meter similar to FIG. 3 sections 305 , 306 , 307 , 311 , 313 , and 314 . At the same time, electrodes on the meter can make contact with the electrodes on the electrochemical test strip, again allowing simultaneous glucose and backscattering turbidity measurements to be performed.
A particularly simple test strip configuration, somewhat favored due to the lower manufacturing cost, is shown in FIG. 10 . FIG. 10 shows a “sandwich” type electrochemical blood glucose test strip, similar to that previously shown in FIG. 4 , with two fiber-optic fibers 1001 and 1003 accessing the central cavity 109 . Near infrared light 1000 from the external meter (not shown) enters central cavity 109 through fiber end 1002 . In this configuration, optical fiber end 1002 is usually not tipped with any reagent. This light illuminates central cavity 109 . When a drop of blood is applied, it enters into cavity 109 by capillary action, and an electrochemical blood glucose reaction is performed as previously described. At the same time, chylomicrons in the blood sample scatter the light emitted by optical fiber end 1002 . The roughly 180° backscattered light enters optical fiber 1003 by optical fiber end 1004 . This backscattered light 1005 exits optical fiber 1003 , is then analyzed by the external meter's photodetector, and is typically converted by a program running on the external meter's microprocessor into a clinically useful result indicating the extent of lipemia in the blood sample, using an equation such as equation 1.
To test configuration 10 , a simple experiment can be done using a 2 kilohertz pulsed 850 μm LED fiber optic light source (RIFOCS 252A, Rifocs corporation [now Tempo Research Corporation], Camarillo, Calif.), a fiber optic power meter (RIFOCS 575L), and a fiber optic jumper. The fiber optic jumper is broken in the middle, the two fiber optic strands exposed and placed 1 mm apart on a 10-mil thick plastic sheet in a backscattering configuration (both fibers parallel with each other and pointing in the same direction). The apparatus can be challenged with a drop of whole blood obtained from a patient after a 12 hour fast, and with a drop of whole blood obtained from a patient 3 hours after eating an extremely fatty meal. The light scattering signal from the patients can then be detected on the RIFOCS 575L power meter. Typically the light scattering signal obtained from the blood of a fasting patient, as detected by the RIFOCS power meter, will be much less than the light scattering signal obtained from a postprandial lipemic patient.
Still another alternate configuration utilizes evanescent light. It is well known that light traveling through optical fibers penetrates several hundred nanometers beyond the border of the fiber into the outside medium. If the surrounding medium, which in this application will normally be whole blood, does not absorb or scatter the evanescent light, then the light will continue to travel through the fiber with undiminished intensity. However if the surrounding medium contains a high enough density of light scattering particles that come within the several hundred nanometer evanescent zone surrounding the optical fiber, then the intensity of light will be diminished, and a higher amount of light will leak out into the surrounding medium. This scattered light may in turn be captured by a nearby light pipe, and returned to the external meter for subsequent photometric light scattering analysis. | Diagnostic dry reagent tests capable of reacting with a single drop of whole blood and reporting both glucose and light-scattering analytes, such as chylomicrons, are taught. Such dry reagent tests may employ electrochemical detection methodologies, optical detection methodologies, or both methodologies. These tests alert diabetics to excessive levels of postprandial lipemia caused by meals with excessive amounts of fat, and thus can help reduce the risk of cardiovascular complications in diabetic patients. | 2 |
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application is a divisional of U.S. application Ser. No. 12/787,548, filed on May 26, 2010, now pending, which is a continuation-in-part of U.S. application Ser. No. 12/342,104, filed on Dec. 23, 2008, issued as U.S. Pat. No. 7,754,729, on Jul. 13, 2010, which is a continuation of Int'l Pat. Appl. No. PCT/CN2007/001920 filed on Jun. 19, 2007. This Application also claims foreign priority benefits to Chinese Pat. Appl. Nos. 200610014690.1 filed on Jul. 5, 2006 and 200610138377.9 filed on Nov. 10, 2006. The contents of all of the aforementioned Applications, including any intervening amendments thereto, are incorporated herein by reference in their entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The invention relates to a method of preparation of quinazoline and quinoline derivatives, and a method of using the same as pharmaceutical agents.
[0004] 2. Description of the Related Art
[0005] Protein tyrosine kinases (PTKs) modulate a wide variety of cellular events, including differentiation, growth, metabolism, and apoptosis. Transmembrane receptor tyrosine kinases (RTKs), members of the PTK family, are the high affinity cell surface receptors for many polypeptide growth factors, cytokines and hormones.
[0006] The mechanisms by which most RTKs transmit signals are now well established. Binding of ligand results in the dimerization of receptor monomers followed by transphosphorylation of tyrosine residues within the cytoplasmic domains of the receptors. However, mutations in the transmembrane (TM) domains of RTKs have been implicated in the induction of pathological phenotypes. These mutations are believed to stabilize the RTK dimers, and thus promote unregulated signaling without ligand binding.
[0007] Overexpression of PTK in cells can cause weak signals to be amplified. Furthermore, during many steps of cellular signal transfer, the occurrence of mutations or overexpression of PTK can cause false signals. These false signals play a role in carcinogenesis.
[0008] Epidermal growth factor receptor (EGFR) is one of the typical examples. EGFR belongs to cell surface receptors of epidermal growth factor receptor tyrosine kinase (EGFR-TK). The receptor family comprises EGF receptor (a protein product of oncogene erbB-1), erbB-2 (c-neu or HER2) receptor, tumor protein mutant erbB-3 receptor, and erbB-4 receptor. EGF and transforming growth factor alpha (TGFα) are the two most important ligands of EGFR. Though the receptor plays a minor role in healthy adults, it is closely related to the pathological process of most cancers, particularly to colon cancer and breast cancer. Therefore, an EGFR-TK inhibitor that can block the transfer of these receptor signals can be used to treat cancers caused by EGFR overexpression, such as colorectal cancer, breast cancer, kidney cancer, lung cancer, and head and neck cancer.
[0009] An EGFR-TK inhibitor can also be used to treat other diseases caused by EGFR overexpression, such as psoriasis, nephritis and pancreatitis which are described below.
[0010] Conventional treatments for proliferative skin diseases such as psoriasis include anti-cancer drugs, such as methotrexate. However, methotrexate has strong side effects and response is poor within the necessary limited dosage. In psoriatic tissues, TGFα is the main growth factor that is overexpressed. In animal experiments, 50% of transgenic mice with TGFα overexpression produce psoriasis, which suggests that a good inhibitor of EGFR signal transfer mechanism may inhibit psoriasis, i.e., the EGFR-TK inhibitor can relieve psoriasis symptoms.
[0011] EGF is an important epithelial mitogen and plays a role in renal tubular cell replication. In streptozotocin-induced diabetic mice, secretion of urine and mRNA of EGF are increased fourfold. Additionally, the expression of EGFR is enhanced in patients with proliferative glomerulonephritis (Roy-Chaudhury et al., Pathology, 1993, 25, 327-332). These findings indicate blocking EGF singal transfer can be used to treat and prevent renal injury. Therefore, it is postulated that an EGFR-TK inhibitor could be used to treat proliferative glomerulonephritis and renal disease induced by diabetes.
[0012] It has been reported that in chronic pancreatitis patients the expression of EGFR and TGFα is much higher than in healthy adults (Korc et al., Gut, 1994, 35, 1468). The overexpression of erbB-2 receptor has been confirmed in patients with severe chronic pancreatitis (Friess et al., Ann. Surg., 1994, 220, 183). Therefore, it is postulated that an EGFR-TK inhibitor could potentially be used to treat pancreatitis.
[0013] During embryonic cell maturation, embryonic cell implantation in endometrium, and other peripheral implantation, EGF and TGFα are present in uterine tissues (Taga, Nippon Sanka Fujinka Gakkai Zasshi, 1992, 44, 939) and EGFR levels are increased (Brown et al., Endocrinology, 1989, 124, 2882). Meanwhile, heparin-binding EGF (HB-EGF) is expressed in the uterus in a blastocyst-mediated process. (Das et al, Development, 1994, 120, 1071). TGFα and EGFR are highly expressed in embryonic cells (Adamson, Mol. Reprod. Dev., 1990, 27, 16). Surgical removal the submandibular gland and treatment with monoclonal antibody against EGFR can greatly reduce the fertility of mice by decreasing the success of embryonic cell implantation (Tsutsumi et al., J. Endocrinology, 1993, 138, 437). These results indicate that an EGFR-TK inhibitor may function as a contraceptive.
[0014] WO1992/007844 and WO1992/014716 disclose 2,4-diaminoquinazoline derivatives which are used as potentiators of chemotherapeutic agents in the treatment of cancer.
[0015] WO1992/020642 discloses bis mono- and bicyclic aryl and heteroaryl compounds which inhibit EGF and/or PDGF receptor tyrosine kinase.
[0016] EP520722, EP566226, EP635498, EP602851, WO 1995/019774 and WO 1995/15758 relate to reversible EGF receptor tyrosine kinase inhibitors. These inhibitors belong to the family of aryl and heteroaryl quinazoline derivatives and some exhibit a high inhibitory activity against EGF receptor tyrosine kinase. However, in animal pathological models these inhibitors exhibit low activity. The reason for this lies in that PTK is a catalyst catalyzing a phosphate group to transfer from ATP to a protein tyrosine residue, and the above-mentioned reversible EGF receptor tyrosine kinase inhibitors compete with ATP to bind EGF receptor tyrosine kinase, but in cells the ATP concentration is much higher (mM grade). Thus, the reversible EGF receptor tyrosine kinase inhibitors exhibiting a high activity in vitro have difficulty functioning in pathological animal models. However, since irreversible EGF receptor tyrosine kinase inhibitors do not compete with ATP, they are expected to do better in vivo.
[0017] Irreversible EGF receptor tyrosine kinase inhibitors are known and much effort has been devoted to their development. One type of irreversible EGF receptor tyrosine kinase inhibitors features a Michael acceptor at the sixth position of quinazoline, so that a Michael addition reaction can occur between the inhibitor and cysteine sulfhydryl in the active center pocket wall of EGF receptor tyrosine kinase. Furthermore, the activity of the inhibitor has a positive correlation with the activation energy of the Michael addition reaction between the inhibitor and cysteine sulfhydryl.
SUMMARY OF THE INVENTION
[0018] In view of the above-described problems, it is an objective of the invention to provide a compound or pharmaceutically acceptable salt or hydrate thereof which can inhibit protein tyrosine kinase activity.
[0019] It is another objective of the invention to provide a pharmaceutical preparation comprising an excipient and a compound or pharmaceutically acceptable salt or hydrate thereof which inhibits protein tyrosine kinase activity.
[0020] It is still another objective of the invention to provide a method of preparing a compound which irreversibly inhibits protein tyrosine kinase activity.
[0021] To achieve the above objectives, in accordance with one embodiment of the invention, provided is a compound of formula (I),
[0000]
[0000] wherein X represents N, C—CN, or CH; Y represents CH 2 , S, O or N—R 9 ; R 1 , R 3 , R 7 and R 8 independently represent H, CF 3 , or C 1-6 alkyl; R 2 represents a group selected from formula (II), (III), (IV), (V), (VI), (VII) or (VIII);
[0000]
[0000] R 4 and R 6 independently represent H, C 1-6 alkyl, OC 1-6 alkyl, OH, F, Cl, Br, OCF 3 , or trifluoromethyl; R 5 is independently at each occurrence selected from H, F, C 1-6 alkyl, OH, OC 1-6 alkyl, OCF 3 , OCF 2 CH 3 , NH 2 , NH(C 1-6 alkyl), N(C 1-6 alkyl) 2 , 1-pyrrolinyl, 1-piperidyl, 4-morpholinyl, Cl, Br, trifluoromethyl, O(CH 2 ) 2-4 OCF 3 , O(CH 2 ) 2-4 OC 1-6 alkyl, O(CH 2 ) 2-4 NH(C 1-6 alkyl), O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 2-4 O, (1-piperidyl)(CH 2 ) 2-4 O, (4-morpholinyl)(CH 2 ) 2-4 O, NHC(O)H, NHC(O)(C 1-6 alkyl), N(C 1-6 alkyl)C(O)(C 1-6 alkyl), O(CH 2 ) 2-4 OH, N(C 1-6 alkyl)C(O)O(C 1-6 alkyl), N(C 1-6 alkyl)C(O)OH, NHC(O)O(C 1-6 alkyl), OC(O)NH(C 1-6 alkyl), OC(O)N(C 1-6 alkyl) 2 , (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-imidazolyl)(CH 2 ) 2-4 O, (4-imidazolyl)(CH 2 ) 2-4 OC(O), (pyrazolyl)(CH 2 ) 2-4 O, (triazolyl)(CH 2 ) 2-4 OC(O) or Ar(CH 2 ) 1-4 O; R 9 at each occurrence is independently selected from H, C 1-6 alkyl, CF 3 , CF 2 CH 3 , (CH 2 ) 2-4 OH, (CH 2 ) 1-4 OC 1-6 alkyl, (CH 2 ) 1-4 NH(C 1-6 alkyl), (CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-4 , (1-piperidyl)(CH 2 ) 1-4 , (4-morpholinyl)(CH 2 ) 1-4 , C(O)C 1-6 alkyl, C(O)(CH 2 ) 1-4 OH, C(O)(CH 2 ) 1-4 OC 1-6 alkyl, C(O)(CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-6 C(O), (1-piperidyl)(CH 2 ) 1-6 C(O), (4-morpholinyl)(CH 2 ) 1-4 C(O), C(O)OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , C(O)O(CH 2 ) 2-4 NH(C 1-6 alkyl), (1-pyrrolinyl) (CH 2 ) 2-4 OC(O), (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (CH 2 ) 1-4 C(O)OC 1-6 alkyl, or Ar(CH 2 ) 1-4 ; R 10 represents H, C 1-6 alkyl, or F; R 11 and R 12 represent independently at each occurrence H, F, Cl, Br, I, CN, NO 2 , CF 3 , OH, NH 2 , C 1-4 alkyl, OC 1-4 alkyl, OCF 3 , OCF 2 CH 3 , NH(C 1-4 alkyl), N(C 1-4 alkyl) 2 , OC(O)C 1-4 alkyl, NHC(O)H, NHC(O)C 1-4 alkyl, N(C 1-4 alkyl)C(O)C 1-4 alkyl, C(O)OC 1-4 alkyl, C(O)NHC 1-4 alkyl, C(O)N(C 1-4 alkyl) 2 , COOH, C(O)C 1-4 alkyl, S(O)C 1-4 alkyl, SO 2 C 1-4 alkyl, SO 2 NHC 1-4 alkyl or SO 2 N(C 1-4 alkyl) 2 ; A, B independently represent aromatic ring; Ar is phenyl, substituted phenyl, or pyridyl; D represents O, S, NH, or methylene; m, n independently represent an integer from 0 to 4; z is 0, 1, or 2; and t and u independently represent an integer from 0 to 4.
[0022] As used herein the term “substituted phenyl” means phenyl substituted by one or more substituents selected from phenyl substituted by one or more halo, C 1-8 alkyl, C 1-8 alkoxy, carboxyl, C 1-8 haloalkyl, C 1-8 alkylthio, phenyl, nitro, amino, C 1-8 alkylcarboxylamino, hydroxyl, acetyl, acetyloxy, phenoxy; C 1-8 alkoxycarbonyl, or C 1-8 alkylcarbonyl.
[0023] In the embodiments of the invention, C 1-4 alkyl and C 1-6 alkyl are straight chain alkyl, branched chain alkyl, or cyclic alkyl, saturated or unsaturated alkyl, optionally substituted with F, OH, COOH, CO 2 (C 1-4 alkyl), C(O)NH 2 , C(O)NH(C 1-4 alkyl), C(O)N(C 1-4 alkyl) 2 , NHC(O)(C 1-4 alkyl), NH 2 , NH(C 1-4 alkyl), N(C 1-4 alkyl) 2 , NHC(O)NH 2 , NHC(NH)NH 2 , O(C 1-4 alkyl), or S(C 1-4 alkyl).
[0024] When A, B independently represent an aromatic ring, the ring is a 5 to 7-membered and contains from 0 to 4 heteroatoms, such as N, O or S. A, B can also independently represent a polycyclic aromatic group consisting of two or three 5 to 7-membered fused rings.
[0025] In the embodiments of the invention, the connecting position of the group R 2 connected to the amine group of the fourth position of the mother nucleus is not limited to the position as shown by the broken line, other position is also applicable.
[0026] When the compound of formula (I) is defined as an E/Z isomer, it can be an E isomer or a Z isomer or a mixture of an E isomer and a Z isomer.
[0027] When the compound of formula (I) is defined as an R/S isomer, it can be an R isomer, or an S isomer, or a mixture of an R isomer and an S isomer.
[0028] The uniqueness of the compound of the invention is clearly visualized by comparing the structure and property of the compound of Example 33 with the comparison compound A of Example 84, compound B of Example 85 and compound C.
[0000]
[0029] The comparison compound C is an irreversible small molecular EGFR-TK inhibitor having the highest activity among all literature-reported compounds. At a molecular level, the EC 50 value of the comparison compound C against EGFR-TK is 10 −7 μM, while in the same test EC 50 value of the comparison compound B is merely about 0.5 μM, which means the activity of the comparison compound B is five million times lower compared to the comparison compound C. The difference between the two compounds in chemical structure is merely the difference in the steric hindrance of substituted branch of the sixth position. Based on that rule, the activity of the compound of the invention should be lower than that of the comparison compound B.
[0030] However, in a test of inhibitory activity of EGFR-TK at cellular level, the activity of the compound of the invention was unexpectedly several orders of magnitude higher than that of the comparison compound B. For example, the activity of the compound in Example 33 is not only much higher than that of the comparison compound B, but also close to the comparison compound A (as shown in Table 3, 4). However, the EC 50 value of the comparison compound A and C against EGFR-TK is equivalent at the molecular level, which means that the activity of the compound in Example 33 is equivalent to that of the comparison compound C, and it is a million times higher than that of the comparison compound B.
[0031] It has been reported in the literature that the activity of an irreversible EGFR-TK inhibitor is ten times higher than that of a reversible EGFR-TK inhibitor in A431 animal tumor model, but that the activity of the two is equivalent at a molecular level. The compound of the present invention is proven to be an irreversible EGFR-TK inhibitor by a cellular model test (as shown in Table 5), while the high activity comparison compound A to be a reversible inhibitor in the same test, which conforms to the results of a direct test using EGFR-TK described in the literature.
[0032] The compounds of the invention also inhibit Her-2 TK, and part of the results are listed in Table 6.
[0033] The compounds of the invention show a certain degree of growth inhibition against epidermal cancer cell strain A431, colorectal cancer cell strain LoVo, breast cancer cell strain BT 474 and breast cancer cell strain SK-Br-3. A part of the test results are listed in Tables 7, 8 and 9. Some compounds have 30 times higher growth-inhibition activities against A431 than Tarceva (as shown in Table 7). Some compounds have equivalent growth-inhibition activities against breast cancer with Lapatinib (as shown in Table 8). Some have better growth-inhibition activities against colorectal cancer cell LoVo than adriamycin (as shown in Table 9).
[0034] Accordingly, the invention teaches a method of inhibiting cancer cell growth in mammals comprising administering to a mammal in need thereof the compound of formula (I) or pharmaceutically acceptable salt or hydrate thereof, wherein the cancer includes but is not limited to breast cancer, skin cancer, colorectal cancer, head and neck cancer, lung cancer, kidney cancer, bladder cancer, ovarian cancer, oral cancer, laryngeal cancer, esophageal cancer, gastric cancer, cervical cancer, or liver cancer.
[0035] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 1 represents H, CH 3 , or CH 2 CH 3 , more particularly R 1 represents H.
[0036] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 3 represents H, CH 3 or CH 2 CH 3 , more particularly R 3 represents H.
[0037] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 7 represents H, CH 3 or CH 2 CH 3 , more particularly R 7 represents H.
[0038] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 8 represents H, CH 3 or CH 2 CH 3 , more suitably R 8 represents H.
[0039] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 4 represents H, F, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , OCH 3 , or OCH 2 CH 3 ; more particularly, R 4 represents H, F, CH 3 , CH 2 CH 3 or OCH 3 ; and most particularly, R 4 represents H, F, CH 3 , or OCH 3 .
[0040] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 6 represents H, F, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , OCH 3 , OCF 3 or OCH 2 CH 3 ; more particularly, R 6 represents H, F, CH 3 , CH 2 CH 3 or OCH 3 ; and most particularly, R 6 represents H, F, CH 3 , or OCH 3 .
[0041] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein A represents benzene ring, pyridine, pyrimidine, pyrazine, 4-nitrogen heterocyclic pyridine, pyrrole, furan, thiophene, pyrazole, thiazole, indole, benzofuran, benzothiophene, or naphthalene ring; more particularly, A represents benzene ring, pyridine, thiophene, pyrazole, thiazole, indole, or naphthalene ring.
[0042] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein B represents benzene ring, pyridine, pyrimidine, pyrazine, 4-nitrogen heterocyclic pyridine, pyrrole, furan, thiophene, pyrazole, thiazole, indole, benzofuran, benzothiophene or naphthalene ring; and more particularly, B represents benzene ring, pyridine, thiophene, pyrazole, thiazole, indole, or naphthalene ring.
[0043] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein D represents O, S, or NH; more particularly, D represents O.
[0044] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 10 represents H, F, CH 3 , CF 3 , or Et, and z is 0, 1, or 2; more particularly, R 10 represents H, F, CH 3 , or CF 3 , and z is 0, 1 or 2; and most particularly, z is 0.
[0045] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 11 represents independently at each occurrence H, F, Cl, Br, CN, NO 2 , CF 3 , OH, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , alkynyl, OCH 3 , OCH 2 CH 3 , OCF 3 , CO 2 CH 3 , CO 2 CH 2 CH 3 , NH 2 , NHCH 3 , NHCH 2 CH 3 , N(CH 3 ) 2 , NHC(O)H, NHC(O)CH 3 , NHC(O)CH 2 CH 3 , N(CH 3 )C(O)CH 3 , C(O)NHCH 3 , C(O)NHCH 2 CH 3 or C(O)N(CH 3 ) 2 ; more particularly, R 11 represents independently at each occurrence H, F, Cl, Br, CN, CF 3 , OH, CH 3 , CH 2 CH 3 , ethynyl, OCH 3 , OCH 2 CH 3 , OCF 3 , CO 2 CH 3 , CO 2 CH 2 CH 3 , NH 2 , NHCH 3 , NHCH 2 CH 3 , N(CH 3 ) 2 or NHC(O)CH 3 , most particularly, R 11 represents independently at each occurrence H, F, Cl, Br, CN, CF 3 , CH 3 , CH 2 CH 3 , ethynyl, OCH 3 , OCH 2 CH 3 , OCF 3 , CO 2 CH 2 CH 3 , NH 2 , NHCH 3 , NHCH 2 CH 3 , N(CH 3 ) 2 , or NHC(O)CH 3 .
[0046] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein t is an integer from 1 to 4; and more particularly t is 1 or 2.
[0047] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 12 represent independently at each occurrence H, F, Cl, Br, CN, NO 2 , CF 3 , OH, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , alkynyl, OCH 3 , OCH 2 CH 3 , OCF 3 , CO 2 CH 3 , CO 2 CH 2 CH 3 , NH 2 , NHCH 3 , NHCH 2 CH 3 , N(CH 3 ) 2 , NHC(O)H, NHC(O)CH 3 , NHC(O)CH 2 CH 3 , N(CH 3 )C(O)CH 3 , C(O)NHCH 3 , C(O)NHCH 2 CH 3 or C(O)N(CH 3 ) 2 ; and more particularly, R 12 represent independently at each occurrence H, F, Cl, Br, CN, CF 3 , OH, CH 3 , CH 2 CH 3 , ethynyl, OCH 3 , OCH 2 CH 3 , OCF 3 , CO 2 CH 3 , CO 2 CH 2 CH 3 , NH 2 , NHCH 3 , NHCH 2 CH 3 , N(CH 3 ) 2 , or NHC(O)CH 3 .
[0048] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein u is an integer from 1 to 4; and more particularly u is 1 or 2.
[0049] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 5 is independently at each occurrence selected from H, F, OH, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , OCH 3 , OCH 2 CH 3 , OCF 3 , OCF 2 CH 3 , NH 2 , NHCH 3 , N(CH 3 ) 2 , 1-pyrrolinyl, 1-piperidyl, 4-morpholinyl, trifluoromethyl, O(CH 2 ) 2 OH, O(CH 2 ) 3 OH, O(CH 2 ) 4 OH, O(CH 2 ) 2 OCH 3 , O(CH 2 ) 3 OCH 3 , O(CH 2 ) 4 OCH 3 , O(CH 2 ) 2 OCH 2 CH 3 , O(CH 2 ) 3 OCH 2 CH 3 , O(CH 2 ) 4 OCH 2 CH 3 , O(CH 2 ) 2 N(CH 3 ) 2 , O(CH 2 ) 3 N(CH 3 ) 2 , O(CH 2 ) 4 N(CH 3 ) 2 , O(CH 2 ) 2 N(CH 2 CH 3 ) 2 , O(CH 2 ) 3 N(CH 2 CH 3 ) 2 , O(CH 2 ) 4 N(CH 2 CH 3 ) 2 , O(CH 2 ) 2 N(CH 3 )CH 2 CH 3 , O(CH 2 ) 3 N(CH 3 )CH 2 CH 3 , O(CH 2 ) 4 N(CH 3 )CH 2 CH 3 , O(CH 2 ) 2 NH(CH 3 ), O(CH 2 ) 3 NH(CH 3 ), O(CH 2 ) 4 NH(CH 3 ), (1-pyrrolinyl)(CH 2 ) 2 O, (1-pyrrolinyl)(CH 2 ) 3 O, (1-pyrrolinyl)(CH 2 ) 4 O, (1-piperidyl)(CH 2 ) 2 O, (1-piperidyl) (CH 2 ) 3 O, (1-piperidyl)(CH 2 ) 4 O, (4-morpholinyl)(CH 2 ) 2 O, (4-morpholinyl)(CH 2 ) 3 O, (4-morpholinyl)(CH 2 ) 4 O, NHC(O)H, NHC(O)CH 3 , NHC(O)CH 2 CH 3 , NHC(O)CH 2 CH 2 CH 3 , N(CH 3 )C(O)H, N(CH 3 )C(O)CH 3 , N(CH 3 )C(O)CH 2 CH 3 , N(CH 3 )C(O)CH 2 CH 2 CH 3 , NHC(O)OCH 3 , NHC(O)OCH 2 CH 3 , N(CH 3 )C(O)OCH 3 , N(CH 3 )C(O)OCH 2 CH 3 , N(CH 3 )C(O)OCH 2 CH 2 CH 3 , OC(O)NHCH 3 , OC(O)NHCH 2 CH 3 , OC(O)N(CH 3 ) 2 , or OC(O)N(CH 3 )CH 2 CH 3 .
[0050] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein R 9 is independently at each occurrence selected from H, CH 3 , CH 2 CH 3 , CH 2 CH 2 CH 3 , CF 3 , CF 2 CH 3 , (CH 2 ) 2 OH, (CH 2 ) 3 OH, (CH 2 ) 4 OH, (CH 2 ) 2 OCH 3 , (CH 2 ) 3 OCH 3 , (CH 2 ) 4 OCH 3 , (CH 2 ) 2 OCH 2 CH 3 , (CH 2 ) 3 OCH 2 CH 3 , (CH 2 ) 4 OCH 2 CH 3 , (CH 2 ) 2 N(CH 3 ) 2 , (CH 2 ) 3 N(CH 3 ) 2 , (CH 2 ) 4 N(CH 3 ) 2 , (CH 2 ) 2 N(CH 2 CH 3 ) 2 , (CH 2 ) 3 N(CH 2 CH 3 ) 2 , (CH 2 ) 4 N(CH 2 CH 3 ) 2 , (CH 2 ) 2 N(CH 3 )CH 2 CH 3 , (CH 2 ) 3 N(CH 3 )CH 2 CH 3 , (CH 2 ) 4 N(CH 3 )CH 2 CH 3 , (CH 2 ) 2 NH(CH 3 ), (CH 2 ) 3 NH(CH 3 ), (CH 2 ) 4 NH(CH 3 ), (1-pyrrolinyl)(CH 2 ) 2 —, (1-pyrrolinyl)(CH 2 ) 3 —, (1-pyrrolinyl)(CH 2 ) 4 —, (1-piperidyl)(CH 2 ) 2 —, (1-piperidyl)(CH 2 ) 3 , (1-piperidyl)(CH 2 ) 4 , (4-morpholinyl)(CH 2 ) 2 , (4-morpholinyl)(CH 2 ) 3 , (4-morpholinyl)(CH 2 ) 4 , C(O)CH 3 , C(O)CH 2 CH 3 , C(O)CH 2 CH 2 CH 3 , C(O)(CH 2 ) 4 OH, C(O)CH 2 OH, C(O)(CH 2 ) 2 OH, C(O)(CH 2 ) 3 OH, C(O)CH 2 OCH 3 , C(O)(CH 2 ) 2 OCH 3 , C(O)(CH 2 ) 3 OCH 3 , C(O)(CH 2 ) 4 OCH 3 , C(O)CH 2 OCH 2 CH 3 , C(O)CH 2 N(CH 3 ) 2 , C(O)(CH 2 ) 2 N(CH 3 ) 2 , C(O)(CH 2 ) 3 N(CH 3 ) 2 , C(O)(CH 2 ) 4 N(CH 3 ) 2 , C(O)CH 2 N(CH 3 )CH 2 CH 3 , C(O)(CH 2 ) 2 N(CH 3 )CH 2 CH 3 , C(O)(CH 2 ) 3 N(CH 3 )CH 2 CH 3 , C(O)(CH 2 ) 4 N(CH 3 )CH 2 CH 3 , C(O)CH 2 NHCH 2 CH 3 , C(O)(CH 2 ) 2 NHCH 2 CH 3 , C(O)(CH 2 ) 3 NHCH 2 CH 3 , C(O)(CH 2 ) 4 NHCH 2 CH 3 , C(O)CH 2 NHCH 3 , C(O)(CH 2 ) 2 NHCH 3 , C(O)(CH 2 ) 3 NHCH 3 , C(O)(CH 2 ) 4 NHCH 3 , C(O)CH 2 NHPr, C(O)(CH 2 ) 2 NHPr, C(O)(CH 2 ) 3 NHPr, C(O)(CH 2 ) 4 NHPr, C(O)CH 2 N(CH 2 CH 3 ) 2 , C(O)(CH 2 ) 2 N(CH 2 CH 3 ) 2 , C(O)(CH 2 ) 3 N(CH 2 CH 3 ) 2 , C(O)(CH 2 ) 4 N(CH 2 CH 3 ) 2 , (1-pyrrolinyl)CH 2 C(O), (1-pyrrolinyl)(CH 2 ) 2 C(O), (1-pyrrolinyl)(CH 2 ) 3 C(O), (1-pyrrolinyl)(CH 2 ) 4 C(O), (1-piperidyl)CH 2 C(O), (1-piperidyl)(CH 2 ) 2 C(O), (1-piperidyl)(CH 2 ) 3 C(O), (1-piperidyl)(CH 2 ) 4 C(O), (4-morpholinyl)(CH 2 ) 4 C(O), (4-morpholinyl)(CH 2 ) 3 C(O), (4-morpholinyl)CH 2 C(O), (4-morpholinyl)(CH 2 ) 2 C(O), C(O)OCH 3 , C(O)OCH 2 CH 3 , C(O)OPr, C(O)OPr-i, C(O)O(CH 2 ) 2 OCH 3 , C(O)O(CH 2 ) 3 OCH 3 , C(O)O(CH 2 ) 4 OCH 3 , C(O)O(CH 2 ) 2 OCH 2 CH 3 , C(O)O(CH 2 ) 2 N(CH 3 ) 2 , C(O)O(CH 2 ) 3 N(CH 3 ) 2 , C(O)O(CH 2 ) 4 N(CH 3 ) 2 , (1-pyrrolinyl)(CH 2 ) 2 OC(O), (1-pyrrolinyl)(CH 2 ) 3 OC(O), (1-pyrrolinyl)(CH 2 ) 4 OC(O), (1-piperidyl)(CH 2 ) 2 OC(O), (1-piperidyl)(CH 2 ) 3 OC(O), (1-piperidyl)(CH 2 ) 4 OC(O), (4-morpholinyl)(CH 2 ) 2 OC(O), (4-morpholinyl)(CH 2 ) 3 OC(O), (4-morpholinyl)(CH 2 ) 4 OC(O), CH 2 C(O)OCH 3 , (CH 2 ) 2 C(O)OCH 3 , (CH 2 ) 3 C(O)OCH 3 , CH 2 C(O)OCH 2 CH 3 , (CH 2 ) 2 C(O)OCH 2 CH 3 , or (CH 2 ) 3 C(O)OCH 2 CH 3 .
[0051] The compound of formula (I) suitable for being used as medical active ingredient comprises the compounds wherein m and n each independently represent an integer from 0 to 4; and particularly 0, 1 or 2.
[0000]
TABLE 1
Examples of R 9 and R 11 in the compound of formula (I) suitable
for being used as active medical ingredient
R 9
R 11
R 9
R 11
H
H
H
3-Cl
H
3-Br
H
3-F
H
3-CH 3
H
3-CF 3
H
3-alkynyl
H
3-CN
H
3-NO 2
H
3-OCH 3
H
3-C(O)CH 3
H
3-SO 2 CH 3
H
3-S(O)CH 3
H
3-CO 2 CH 3
H
3-SO 2 NHCH 3
H
3-CO 2 CH 2 CH 3
H
3-SO 2 N(CH 3 ) 2
H
3-CONHCH 3
H
3-CON(CH 3 ) 2
H
4-CON(CH 3 ) 2
H
3-I
H
4-Cl
H
4-Br
H
4-F
H
4-CH 3
H
4-CF 3
H
4-alkynyl
H
4-CN
H
4-NO 2
H
4-OCH 3
H
4-C(O)CH 3
H
4-SO 2 CH 3
H
4-S(O)CH 3
H
4-CO 2 CH 3
H
4-SO 2 NHCH 3
H
4-CO 2 CH 2 CH 3
H
4-SO 2 N(CH 3 ) 2
H
4-CONHCH 3
H
4-F-3-Br
H
4-F-3-I
H
4-F-3-CH 3
H
4-F-3-CF 3
H
4-F-3-alkynyl
H
4-F-3-CN
H
4-F-3-NO 2
H
4-F-3-OCH 3
H
4-F-3-C(O)CH 3
H
4-F-3-SO 2 CH 3
H
4-F-3-S(O)CH 3
H
4-F-3-CO 2 CH 3
H
4-F-3-SO 2 NHCH 3
H
4-F-3-CO 2 CH 2 CH 3
H
4-F-3-SO 2 N(CH 3 ) 2
H
4-F-3-CONHCH 3
H
4-F-3-CON(CH 3 ) 2
H
3-F-4-F
H
4-F-3-Cl
CH 3
H
CH 3
3-Cl
CH 3
3-Br
CH 3
3-F
CH 3
3-CH3
CH 3
3-CF 3
CH 3
3-alkynyl
CH 3
3-CN
CH 3
3-NO2
CH 3
3-OCH 3
CH 3
3-C(O)CH 3
CH 3
3-SO 2 CH 3
CH 3
3-S(O)CH 3
CH 3
3-CO 2 CH 3
CH 3
3-SO 2 NHCH 3
CH 3
3-CO 2 CH 2 CH 3
CH 3
3-SO 2 N(CH 3 ) 2
CH 3
3-CONHCH 3
CH 3
3-CON(CH 3 ) 2
CH 3
4-CON(CH 3 ) 2
CH 3
3-I
CH 3
4-Cl
CH 3
4-Br
CH 3
4-F
CH 3
4-CH 3
CH 3
4-CF 3
CH 3
4-alkynyl
CH 3
4-CN
CH 3
4-SO 2 N(CH 3 ) 2
CH 3
4-CONHCH 3
CH 3
4-F-3-Br
CH 3
4-F-3-I
CH 3
4-F-3-CH 3
CH 3
4-F-3-CF 3
CH 3
4-F-3-alkynyl
CH 3
4-F-3-CN
CH 3
4-F-3-NO 2
CH 3
4-F-3-OCH 3
CH 3
4-F-3-C(O)CH 3
CH 3
4-F-3-SO 2 CH 3
CH 3
4-F-3-S(O)CH 3
CH 3
4-F-3-CO 2 CH 3
CH 3
4-F-3-SO 2 NHCH 3
CH 3
4-F-3-CO 2 CH 2 CH 3
CH 3
4-F-3-SO 2 N(CH 3 ) 2
CH 3
4-F-3-CONHCH 3
CH 3
4-F-3-CON(CH 3 ) 2
CH 3
4-F-3-CON(CH 3 ) 2
CH 3
4-F-3-Cl
CH 3
3-F-4-F
CH 3
2-SO 2 CH 3
CH 3
3-COOH
CH 3
4-COOH
CH 3
2-C(O)OCH 3
CH 3
2-I
CH 3
2-Cl
CH 3
2-Br
CH 3
2-F
CH 3
2-CH 3
CH 3
2-CH 3
CH 3
2-alkynyl
CH 3
2-CN
CH 3
2-NO 2
CH 3
2-OCH 3
CH 3
2-C(O)CH 3
Et
3-Cl
Et
3-Br
Et
3-F
Et
3-CH 3
Et
3-CF 3
Et
3-alkynyl
Et
3-CN
Et
3-NO 2
Et
3-OCH 3
Et
3-C(O)CH 3
Et
3-SO 2 CH 3
Et
3-S(O)CH 3
Et
3-CO 2 CH 3
Et
3-SO 2 NHCH 3
Et
3-CO 2 CH 2 CH 3
Et
3-SO 2 N(CH 3 ) 2
Et
3-CONHCH 3
Et
3-CON(CH 3 ) 2
Et
4-CON(CH 3 ) 2
Et
3-I
Et
4-Cl
Et
4-Br
Et
4-F
Et
4-CH 3
Et
4-CF 3
Et
4-alkynyl
Et
4-CN
Et
4-NO 2
Et
4-OCH 3
Et
4-C(O)CH 3
Et
4-SO 2 CH 3
Et
4-S(O)CH 3
Et
4-CO 2 CH 3
Et
4-SO 2 NHCH 3
Et
4-CO 2 CH 2 CH 3
Et
4-SO 2 N(CH 3 ) 2
Et
4-CONHCH 3
Et
4-F-3-Br
Et
4-F-3-I
Et
4-F-3-CH 3
Et
4-F-3-CF 3
Et
4-F-3-alkynyl
Et
4-F-3-CN
Et
4-F-3-NO 2
Et
4-F-3-OCH 3
Et
4-F-3-C(O)CH 3
Et
4-F-3-SO 2 CH 3
Et
4-F-3-S(O)CH 3
Et
4-F-3-CO 2 CH 3
Et
4-F-3-SO 2 NHCH 3
Et
4-F-3-CO 2 CH 2 CH 3
Et
4-F-3-SO 2 N(CH 3 ) 2
Et
4-F-3-CONHCH 3
Et
4-F-3-CON(CH 3 ) 2
Et
H
Et
4-F-3-Cl
Et
3-F-4-F
Et
2-SO 2 CH 3
Et
3-COOH
Et
4-COOH
Et
2-C(O)OCH 3
Et
2-I
Et
2-Cl
Et
2-Br
Et
2-F
Et
2-CH 3
Et
2-CH 3
Et
2-alkynyl
Et
2-CN
Et
2-NO 2
Et
2-OCH 3
Et
2-C(O)CH 3
(CH 2 ) 2 OMe
3-CON(CH 3 ) 2
(CH 2 ) 2 OMe
H
(CH 2 ) 2 OMe
3-Cl
(CH 2 ) 2 OMe
3-Br
(CH 2 ) 2 OMe
3-F
(CH 2 ) 2 OMe
3-CH 3
(CH 2 ) 2 OMe
3-CF 3
(CH 2 ) 2 OMe
3-alkynyl
(CH 2 ) 2 OMe
3-CN
(CH 2 ) 2 OMe
3-NO 2
(CH 2 ) 2 OMe
3-OCH 3
(CH 2 ) 2 OMe
3-C(O)CH 3
(CH 2 ) 2 OMe
3-SO 2 CH 3
(CH 2 ) 2 OMe
3-S(O)CH 3
(CH 2 ) 2 OMe
3-CO 2 CH 3
(CH 2 ) 2 OMe
3-SO 2 NHCH 3
(CH 2 ) 2 OMe
3-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
3-CONHCH 3
(CH 2 ) 2 OMe
3-I
(CH 2 ) 2 OMe
4-Cl
(CH 2 ) 2 OMe
4-Br
(CH 2 ) 2 OMe
4-F
(CH 2 ) 2 OMe
4-CH 3
(CH 2 ) 2 OMe
4-CF 3
(CH 2 ) 2 OMe
4-alkynyl
(CH 2 ) 2 OMe
4-CN
(CH 2 ) 2 OMe
4-NO 2
(CH 2 ) 2 OMe
4-OCH 3
(CH 2 ) 2 OMe
4-C(O)CH 3
(CH 2 ) 2 OMe
4-SO 2 CH 3
(CH 2 ) 2 OMe
4-S(O)CH 3
(CH 2 ) 2 OMe
4-CO 2 CH 3
(CH 2 ) 2 OMe
4-SO 2 NHCH 3
(CH 2 ) 2 OMe
4-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
4-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
4-CONHCH 3
(CH 2 ) 2 OMe
4-CON(CH 3 )
(CH 2 ) 2 OMe
4-F-3-CON(CH 3 ) 2
(CH 2 ) 2 OMe
4-F-3-Br
(CH 2 ) 2 OMe
4-F-3-I
(CH 2 ) 2 OMe
4-F-3-CH 3
(CH 2 ) 2 OMe
4-F-3-CF 3
(CH 2 ) 2 OMe
4-F-3-alkynyl
(CH 2 ) 2 OMe
4-F-3-CN
(CH 2 ) 2 OMe
4-F-3-NO 2
(CH 2 ) 2 OMe
4-F-3-OCH 3
(CH 2 ) 2 OMe
4-F-3-C(O)CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 CH 3
(CH 2 ) 2 OMe
4-F-3-S(O)CH 3
(CH 2 ) 2 OMe
4-F-3-CO 2 CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 NHCH 3
(CH 2 ) 2 OMe
4-F-3-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
4-F-3-CONHCH 3
(CH 2 ) 2 OMe
4-F-3-Cl
(CH 2 ) 2 OMe
3-F-4-F
(CH 2 ) 2 OMe
2-SO 2 CH 3
(CH 2 ) 2 OMe
3-COOH
(CH 2 ) 2 OMe
4-COOH
(CH 2 ) 2 OMe
2-C(O)OCH 3
(CH 2 ) 2 OMe
2-I
(CH 2 ) 2 OMe
2-Cl
(CH 2 ) 2 OMe
2-Br
(CH 2 ) 2 OMe
2-F
(CH 2 ) 2 OMe
2-CH 3
(CH 2 ) 2 OMe
2-CH 3
(CH 2 ) 2 OMe
2-alkynyl
(CH 2 ) 2 OMe
2-CN
(CH 2 ) 2 OMe
2-NO 2
(CH 2 ) 2 OMe
2-OCH 3
(CH 2 ) 2 OMe
2-C(O)CH 3
(CH 2 ) 2 OMe
3-Cl
(CH 2 ) 2 OMe
3-Br
(CH 2 ) 2 OMe
3-F
(CH 2 ) 2 OMe
3-CH 3
(CH 2 ) 2 OMe
3-CF 3
(CH 2 ) 2 OMe
3-alkynyl
(CH 2 ) 2 OMe
3-CN
(CH 2 ) 2 OMe
3-NO 2
(CH 2 ) 2 OMe
3-OCH 3
(CH 2 ) 2 OMe
3-C(O)CH 3
(CH 2 ) 2 OMe
3-SO 2 CH 3
(CH 2 ) 2 OMe
3-S(O)CH 3
(CH 2 ) 2 OMe
3-CO 2 CH 3
(CH 2 ) 2 OMe
3-SO 2 NHCH 3
(CH 2 ) 2 OMe
3-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
3-CONHCH 3
(CH 2 ) 2 OMe
3-CON(CH 3 ) 2
(CH 2 ) 2 OMe
4-CON(CH 3 ) 2
(CH 2 ) 2 OMe
3-I
(CH 2 ) 2 OMe
4-Cl
(CH 2 ) 2 OMe
4-Br
(CH 2 ) 2 OMe
4-F
(CH 2 ) 2 OMe
4-CH 3
(CH 2 ) 2 OMe
4-CF 3
(CH 2 ) 2 OMe
4-alkynyl
(CH 2 ) 2 OMe
4-CN
(CH 2 ) 2 OMe
4-NO 2
(CH 2 ) 2 OMe
4-OCH 3
(CH 2 ) 2 OMe
4-C(O)CH 3
(CH 2 ) 2 OMe
4-SO 2 CH 3
(CH 2 ) 2 OMe
4-S(O)CH 3
(CH 2 ) 2 OMe
4-CO 2 CH 3
(CH 2 ) 2 OMe
4-SO 2 NHCH 3
(CH 2 ) 2 OMe
4-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
4-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
4-CONHCH 3
(CH 2 ) 2 OMe
4-F-3-alkynyl
(CH 2 ) 2 OMe
4-F-3-CN
(CH 2 ) 2 OMe
4-F-3-Br
(CH 2 ) 2 OMe
4-F-3-I
(CH 2 ) 2 OMe
4-F-3-CH 3
(CH 2 ) 2 OMe
4-F-3-CF 3
(CH 2 ) 2 OMe
4-F-3-NO 2
(CH 2 ) 2 OMe
4-F-3-OCH 3
(CH 2 ) 2 OMe
4-F-3-C(O)CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 CH 3
(CH 2 ) 2 OMe
4-F-3-S(O)CH 3
(CH 2 ) 2 OMe
4-F-3-CO 2 CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 NHCH 3
(CH 2 ) 2 OMe
4-F-3-CO 2 CH 2 CH 3
(CH 2 ) 2 OMe
4-F-3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OMe
4-F-3-CONHCH 3
(CH 2 ) 2 OMe
4-F-3-CON(CH 3 ) 2
(CH 2 ) 2 OMe
4-F-3-Cl
(CH 2 ) 2 OMe
3-F-4-F
(CH 2 ) 2 OMe
2-SO 2 CH 3
(CH 2 ) 2 OMe
H
(CH 2 ) 2 OMe
3-COOH
(CH 2 ) 2 OMe
4-COOH
(CH 2 ) 2 OMe
2-C(O)OCH 3
(CH 2 ) 2 OMe
2-I
(CH 2 ) 2 OMe
2-Cl
(CH 2 ) 2 OMe
2-Br
(CH 2 ) 2 OMe
2-F
(CH 2 ) 2 OMe
2-CH 3
(CH 2 ) 2 OMe
2-CF 3
(CH 2 ) 2 OMe
2-alkynyl
(CH 2 ) 2 OMe
2-CN
(CH 2 ) 2 OMe
2-NO 2
(CH 2 ) 2 OMe
2-OCH 3
(CH 2 ) 2 OMe
2-C(O)CH 3
(CH 2 ) 2 OH
3-I
(CH 2 ) 2 OH
H
(CH 2 ) 2 OH
3-Cl
(CH 2 ) 2 OH
3-Br
(CH 2 ) 2 OH
3-F
(CH 2 ) 2 OH
3-CH 3
(CH 2 ) 2 OH
3-CF 3
(CH 2 ) 2 OH
3-alkynyl
(CH 2 ) 2 OH
3-CN
(CH 2 ) 2 OH
3-NO 2
(CH 2 ) 2 OH
3-OCH 3
(CH 2 ) 2 OH
3-C(O)CH 3
(CH 2 ) 2 OH
3-CO 2 CH 3
(CH 2 ) 2 OH
3-S(O)CH 3
(CH 2 ) 2 OH
3-CO 2 CH 2 CH 3
(CH 2 ) 2 OH
3-SO 2 NHCH 3
(CH 2 ) 2 OH
3-CONHCH 3
(CH 2 ) 2 OH
3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OH
4-CON(CH 3 ) 2
(CH 2 ) 2 OH
3-CON(CH 3 ) 2
(CH 2 ) 2 OH
4-Cl
(CH 2 ) 2 OH
4-Br
(CH 2 ) 2 OH
4-F
(CH 2 ) 2 OH
4-CH 3
(CH 2 ) 2 OH
4-CF 3
(CH 2 ) 2 OH
4-alkynyl
(CH 2 ) 2 OH
4-CN
(CH 2 ) 2 OH
4-NO 2
(CH 2 ) 2 OH
4-OCH 3
(CH 2 ) 2 OH
4-C(O)CH 3
(CH 2 ) 2 OH
4-SO 2 CH 3
(CH 2 ) 2 OH
4-S(O)CH 3
(CH 2 ) 2 OH
4-CO 2 CH 3
(CH 2 ) 2 OH
4-SO 2 NHCH 3
(CH 2 ) 2 OH
4-CO 2 CH 2 CH 3
(CH 2 ) 2 OH
4-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OH
4-CONHCH 3
(CH 2 ) 2 OH
4-CON(CH 3 ) 2
(CH 2 ) 2 OH
4-F-3-CON(CH 3 ) 2
(CH 2 ) 2 OH
4-F-3-Br
(CH 2 ) 2 OH
4-F-3-I
(CH 2 ) 2 OH
4-F-3-CH 3
(CH 2 ) 2 OH
4-F-3-CF 3
(CH 2 ) 2 OH
4-F-3-alkynyl
(CH 2 ) 2 OH
4-F-3-CN
(CH 2 ) 2 OH
4-F-3-NO 2
(CH 2 ) 2 OH
4-F-3-OCH 3
(CH 2 ) 2 OH
4-F-3-C(O)CH 3
(CH 2 ) 2 OH
4-F-3-SO 2 CH 3
(CH 2 ) 2 OH
4-F-3-SO 2 NHCH 3
(CH 2 ) 2 OH
4-F-3-CO 2 CH 2 CH 3
(CH 2 ) 2 OH
4-F-3-SO 2 N(CH 3 ) 2
(CH 2 ) 2 OH
4-F-3-CONHCH 3
(CH 2 ) 2 OH
4-F-3-Cl
(CH 2 ) 2 OH
3-F-4-F
(CH 2 ) 2 OH
H
(CH 2 ) 2 OH
3-COOH
(CH 2 ) 2 OH
4-COOH
(CH 2 ) 2 OH
2-C(O)OCH 3
(CH 2 ) 2 OH
2-I
(CH 2 ) 2 OH
2-Cl
(CH 2 ) 2 OH
2-Br
(CH 2 ) 2 OH
2-F
(CH 2 ) 2 OH
2-CH 3
(CH 2 ) 2 OH
2-CH 3
(CH 2 ) 2 OH
2-alkynyl
(CH 2 ) 2 OH
2-CN
(CH 2 ) 2 OH
2-NO 2
(CH 2 ) 2 OH
2-OCH 3
(CH 2 ) 2 OH
2-C(O)CH 3
(CH 2 ) 2 OH
2-SO 2 CH 3
CH 3
4-NO 2
CH 3
4-OCH 3
CH 3
4-C(O)CH 3
CH 3
4-SO 2 CH 3
CH 3
4-S(O)CH 3
CH 3
4-CO 2 CH 3
CH 3
4-SO 2 NHCH 3
CH 3
4-CO 2 CH 2 CH 3
[0000]
TABLE 2
Examples of R 5 in the compound of formula (I) suitable for being used as medical
active ingredient
R 5
R 5
R 5
R 5
F
OH
OCH 3
OCH 2 CH 3
O(CH 2 ) 2 OMe
O(CH 2 ) 3 OMe
O(CH 2 ) 2 OH
OPr-n
OPr-i
O(CH 2 ) 3 OH
O(CH 2 ) 4 OMe
OBu-n
O(CH 2 ) 3 NMe 2
O(CH 2 ) 2 NMe 2
O(CH 2 ) 3 NEt 2
O(CH 2 ) 2 NEt 2
O(CH 2 ) 3 (1-morpholinyl)
O(CH 2 ) 3 (1-pyrrolinyl)
O(CH 2 ) 2 (1-morpholinyl)
O(CH 2 ) 2 (1-pyrrolinyl)
O(CH 2 ) 3 (1-imidazolyl)
O(CH 2 ) 3 (1-piperidyl)
O(CH 2 ) 2 (1-imidazolyl)
O(CH 2 ) 2 (1-imidazolyl)
O(CH 2 ) 4 (1-morpholinyl)
O(CH 2 ) 4 (1-pyrrolyl)
O(CH 2 ) 4 (1-imidazolyl)
H
O(CH 2 ) 4 (1-piperidyl)
CH 3
NMe 2
NHC(O)Me
N(Me)C(O)Me
OCF 3
OCF 2 CH 3
[0052] The invention further relates to a pharmaceutical preparation comprising a pharmaceutically acceptable excipient and a compound of formula (I),
[0000]
[0000] wherein X represents N, C—CN or CH; Y represents CH 2 , S, O or N—R 9 ; R 1 , R 3 , R 7 and R 8 independently represent H, CF 3 , or C 1-6 alkyl; R 2 represents a group selected from formula (II), (III), (IV), (V), (VI), (VII) or (VIII);
[0000]
[0000] R 4 and R 6 independently represent H, C 1-6 alkyl, OC 1-6 alkyl, OH, F, Cl, Br, OCF 3 , or trifluoromethyl; R 5 is independently at each occurrence selected from H, F, C 1-6 alkyl, OH, OC 1-6 alkyl, OCF 3 , O(CH 2 ) 2-4 OCF 3 , OCF 2 CH 3 , NH 2 , NH(C 1-6 alkyl), N(C 1-6 alkyl) 2 , 1-pyrrolinyl, 1-piperidyl, 4-morpholinyl, F, Cl, Br, trifluoromethyl, O(CH 2 ) 2-4 OC 1-6 alkyl, O(CH 2 ) 2-4 NH(C 1-6 alkyl), O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 2-4 O, (1-piperidyl)(CH 2 ) 2-4 O, (4-morpholinyl)(CH 2 ) 2-4 O, NHC(O)H, NHC(O)(C 1-6 alkyl), N(C 1-6 alkyl)C(O)(C 1-6 alkyl), O(CH 2 ) 2-4 OH, N(C 1-6 alkyl)C(O)O(C 1-6 alkyl), N(C 1-6 alkyl)C(O)OH, NHC(O)O(C 1-6 alkyl), OC(O)NH(C 1-6 alkyl), OC(O)N(C 1-6 alkyl) 2 , (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-imidazolyl)(CH 2 ) 2-4 O, (4-imidazolyl)(CH 2 ) 2-4 OC(O), (pyrazolyl)(CH 2 ) 2-4 O, (triazolyl)(CH 2 ) 2-4 OC(O), or Ar(CH 2 ) 1-4 O; R 9 is independently at each occurrence selected from H, C 1-6 alkyl, CF 3 , CF 2 CH 3 , (CH 2 ) 2-4 OH, (CH 2 ) 1-4 OC 1-6 alkyl, (CH 2 ) 1-4 NH(C 1-6 alkyl), (CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-4 , (1-piperidyl)(CH 2 ) 1-4 , (4-morpholinyl)(CH 2 ) 1-4 , C(O)C 1-6 alkyl, C(O)(CH 2 ) 1-4 OH, C(O)(CH 2 ) 1-4 OC 1-6 alkyl, C(O)(CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-6 C(O), (1-piperidyl)(CH 2 ) 1-6 C(O), (4-morpholinyl)(CH 2 ) 1-4 C(O), C(O)OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , C(O)O(CH 2 ) 2-4 NH(C 1-6 alkyl), (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (CH 2 ) 1-4 C(O)OC 1-6 alkyl, or Ar(CH 2 ) 1-4 ; R 10 represents H, C 1-6 alkyl, or F; R 11 and R 12 represent independently at each occurrence H, F, Cl, Br, I, CN, NO 2 , CF 3 , OH, NH 2 , C 1-4 alkyl, OC 1-4 alkyl, OCF 3 , OCF 2 CH 3 , NH(C 1-4 alkyl), N(C 1-4 alkyl) 2 , OC(O)C 1-4 alkyl, NHC(O)H, NHC(O)C 1-4 alkyl, N(C 1-4 alkyl)C(O)C 1-4 alkyl, C(O)OC 1-4 alkyl, C(O)NHC 1-4 alkyl, C(O)N(C 1-4 alkyl) 2 , COOH, C(O)C 1-4 alkyl, S(O)C 1-4 alkyl, SO 2 C 1-4 alkyl, SO 2 NHC 1-4 alkyl, or SO 2 N(C 1-4 alkyl) 2 ; A, B independently represent aromatic ring; Ar is phenyl, substituted phenyl or pyridyl; D represents O, S, NH, or methylene; m and n independently represent an integer from 0 to 4; z is 1, or 2, and t and u independently represent an integer from 0 to 4.
[0053] The pharmaceutical preparation is formulated for a mode of administration selected from oral, intravenous, intraperitoneal, subcutaneous, intramuscular, nasal, ocular, pulmonary, anal, vaginal, or epidermal.
[0054] In other embodiments, this invention relates to treating or preventing physiological disorder caused by EGFR or Her-2 overexpression in mammals comprising administering a compound or a preparation of the invention described herein, the disorder including but not limited to breast cancer, kidney cancer, bladder cancer, oral cancer, laryngeal cancer, esophageal cancer, gastric cancer, colorectal cancer, ovarian cancer, lung cancer, or head and neck cancer. In addition, the application relates to treating or preventing a physiological disorder by inhibiting EGFR-TK activity in mammals, the disorder including but not limited to psoriasis, pneumonia, hepatitis, nephritis, pancreatitis, or diabetes.
[0055] In other aspects of the invention provided is a method for preparing a compound of formula (I),
[0000]
[0000] wherein X represents N, C—CN or CH; Y represents CH 2 , S, O or N—R 9 ; R 1 , R 3 , R 7 and R 8 independently represent H, CF 3 , or C 1-6 alkyl; R 2 represents a group selected from formula (II), (III), (IV), (V), (VI), (VII) or (VIII);
[0000]
[0000] R 4 and R 6 independently represent H, C 1-6 alkyl, OC 1-6 alkyl, OH, F, Cl, Br, OCF 3 , or trifluoromethyl; R 5 is independently at each occurrence selected from H, F, C 1-6 alkyl, OH, OC 1-6 alkyl, OCF 3 , O(CH 2 ) 2-4 OCF 3 , OCF 2 CH 3 , NH 2 , NH(C 1-6 alkyl), N(C 1-6 alkyl) 2 , 1-pyrrolinyl, 1-piperidyl, 4-morpholinyl, F, Cl, Br, trifluoromethyl, O(CH 2 ) 2-4 OC 1-6 alkyl, O(CH 2 ) 2-4 NH(C 1-6 alkyl), O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 2-4 O, (1-piperidyl)(CH 2 ) 2-4 O, (4-morpholinyl)(CH 2 ) 2-4 O, NHC(O)H, NHC(O)(C 1-6 alky), N(C 1-6 alkyl)C(O)(C 1-6 alkyl), O(CH 2 ) 2-4 OH, N(C 1-6 alkyl)C(O)O(C 1-6 alkyl), N(C 1-6 alkyl)C(O)OH, NHC(O)O(C 1-6 alkyl), OC(O)NH(C 1-6 alkyl), OC(O)N(C 1-6 alkyl) 2 , (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-imidazolyl)(CH 2 ) 2-4 O, (4-imidazolyl)(CH 2 ) 2-4 OC(O), (pyrazolyl)(CH 2 ) 2-4 O, (triazolyl)(CH 2 ) 2-4 OC(O), or Ar(CH 2 ) 1-4 O; R 9 is independently at each occurrence selected from H, C 1-6 alkyl, CF 3 , CF 2 CH 3 , (CH 2 ) 2-4 OH, (CH 2 ) 1-4 OC 1-6 alkyl, (CH 2 ) 1-4 NH(C 1-6 alkyl), (CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-4 , (1-piperidyl)(CH 2 ) 1-4 , (4-morpholinyl)(CH 2 ) 1-4 , C(O)C 1-6 alkyl, C(O)(CH 2 ) 1-4 OH, C(O)(CH 2 ) 1-4 OC 1-6 alkyl, C(O)(CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-6 C(O), (1-piperidyl)(CH 2 ) 1-6 C(O), (4-morpholinyl)(CH 2 ) 1-4 C(O), C(O)OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , C(O)O(CH 2 ) 2-4 NH(C 1-6 alkyl), (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (CH 2 ) 1-4 C(O)OC 1-6 alkyl, or Ar(CH 2 ) 1-4 ; R 10 represents H, C 1-6 alkyl, or F; R 11 and R 12 represent independently at each occurrence H, F, Cl, Br, I, CN, NO 2 , CF 3 , OH NH 2 , C 1-4 alkyl, OC 1-4 alkyl, OCF 3 , OCF 2 CH 3 , NH(C 1-4 alkyl), N(C 1-4 alkyl) 2 , OC(O)C 1-4 alkyl, NHC(O)H, NHC(O)C 1-4 alkyl, N(C 1-4 alkyl)C(O)C 1-4 alkyl, C(O)OC 1-4 alkyl, C(O)NHC 1-4 alkyl, C(O)N(C 1-4 alkyl), COOH, C(O)C 1-4 alkyl, S(O)C 1-4 alkyl, SO 2 C 1-4 alkyl, SO 2 NHC 1-4 alkyl, or SO 2 N(C 1-4 alkyl); A, B independently represent aromatic ring; Ar is phenyl, substituted phenyl or pyridyl; D represents O, S, NH, or methylene; m and n independently represent an integer from 0 to 4; z is 1, or 2, and t and u independently represent an integer from 1 to 4; the method comprising the steps of:
[0056] 1) contacting a compound of formula (XI)
[0000]
[0000] with (R 15 )(R 13 )P(O)CH(R 8 )COOR 14 or Ar 3 P═CR 8 CO 2 R 14 to yield a compound of formula (IX)
[0000]
[0000] wherein Y represents CH 2 , S, O, or N—R 9 except NH; R 8 independently represent H, CF 3 , or C 1-6 alkyl; R 9 is independently at each occurrence selected from H, C 1-6 alkyl, CF 3 , CF 2 CH 3 , (CH 2 ) 2-4 OH, (CH 2 ) 1-4 OC 1-6 alkyl, (CH 2 ) 1-4 NH(C 1-6 alkyl), (CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-4 , (1-piperidyl)(CH 2 ) 1-4 , (4-morpholinyl)(CH 2 ) 1-4 , C(O)C 1-6 alkyl, C(O)(CH 2 ) 1-4 OH, C(O)(CH 2 ) 1-4 OC 1-6 alkyl, C(O)(CH 2 ) 1-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 1-6 C(O), (1-piperidyl)(CH 2 ) 1-6 C(O), (4-morpholinyl)(CH 2 ) 1-4 C(O), C(O)OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 OC 1-6 alkyl, C(O)O(CH 2 ) 2-4 N(C 1-6 alkyl) 2 , (1-pyrrolinyl)(CH 2 ) 2-4 OC(O), (1-piperidyl)(CH 2 ) 2-4 OC(O), (4-morpholinyl)(CH 2 ) 2-4 OC(O), (CH 2 ) 1-4 C(O)OC 1-6 alkyl, or Ar(CH 2 ) 1-4 ; R 13 and R 15 are independently C 1-4 alkyl, OC 1-4 -alkyl, phenyl, substituted phenyl, phenoxy, or substituted phenoxy; R 11 represents C 1-5 alkyl; Ar is phenyl or substituted phenyl; and m and n independently represent an integer from 0 to 4.
[0057] 2) the compound of formula (IX) can be firstly transformed into active ester, acyl chloride, acyl imidazole or mixed anhydride and then contacted with the compound of formula (X) to yield a compound of formula (I),
[0000]
[0000] wherein X, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 10 , R 11 , R 12 , A B, D, Ar, m, n, z, t and u are as in claim 1 ; Y represents N—R 9 ; and R 9 is not H. And tertiary amines, such as triethylamine, N-methylmorpholine, trimethylamine, pyridine or substituted pyridine can be used to accelerate the reaction. When the compound of formula (IX) is transformed into acyl chloride, thionyl chloride, phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride, oxalyl chloride, or cyanuric chloride can be used as chlorinating agents.
[0058] Optionally, the compound of formula (IX) can be firstly transformed into anhydride and then contacted with the compound of formula (X), and pyridine or substituted pyridine such as DMAP can be used as catalyst to accelerate the reaction.
[0059] 3) transforming the compound of formula (I), wherein X, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 10 , R 11 , R 12 , A, B, D, Ar, m, n, z, t, and u are as in claim 1 ; Y represents N—R 9 ; and R 9 represents (CH 3 ) 3 OC(O); obtained in step 2) in acidic conditions or pyrrolytic into the compound of formula (XII)
[0000]
[0000] R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 10 , R 11 , R 12 , A, B, D, X, Ar, m, n, z, t and u are as defined in claim 1 ;
[0060] Acidic condition can be achieved by the use of trifluoroacetate acid, hydrochloric acid, sulfonic acid or an acetyl chloride—alcohol system.
[0061] 4) contacting the compound of formula (XII) as defined in step 3) with R 9 -LG to obtain the compound of formula (I), wherein R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , A B, D, X, Y, Ar, m, n, z, t, and u are as defined in claim 1 , and LG represents Cl, Br, I, OMs, or OTs.
[0062] In step 4, organic base such as triethylamine, trimethylamine, pyridine, substituted pyridine or inorganic base such as sodium carbonate, potassium carbonate can be used to accelerate the reaction, and solvent suitable for the reaction comprises acetonitrile, dimethylformamide, dimethylacetamide, tetrahydrofuran, or ethylene glycol dimethyl ether.
[0063] The present invention teaches an irreversible EGF receptor tyrosine kinase inhibitor featuring a unique chemical structure and low reactivity-high inhibitory activity against EGF receptor tyrosine kinase. In one embodiment of the invention, the compound exhibits good inhibitory activity against A431 cell self-phosphorylation stimulated by EGF, and exhibits a certain growth inhibitory activity against the cell strain, and has a good anti-tumor effect in A431 tumor animal pathological model.
DETAILED DESCRIPTION OF THE INVENTION
[0064] Inhibition Experiment of Cellular Epidermal Growth Factor Receptor Tyrosine Kinase
(EGFR-TK)
[0065] 1) A431 cells were cultured in a medium which was prepared by adding 10% FCS into another medium comprising 50% DMEM and 50% F12.
[0066] 2) A431 cells grown in six-well plates were cultured in a serum-free medium for 24 hours. During the 24 hour period the medium was replenished once after 12 hours.
[0067] 3) A solution containing a compound to be assessed was added the A431 cells and the cells were cultured for 2 hours, supplemented twice by a medium free of the compound, and then EGF (100 ng/well) was added, and cultured for 5 minutes.
[0068] 4) A431 cell homogenate was prepared by Laemili buffer which comprised 2% sodium dodecyl sulfonate (SDS), 5% 2-mercaptoethanol, 10% glycerol and 5 mM Tris (pH 6.8).
[0069] 5) The A431 cell homogenate was heated for 5 minutes at 100° C.
[0070] 6) Proteins in the A431 cell homogenates were separated by PAGE and transferred onto a nitrocellulose membrane, and an infrared reading was obtained.
[0071] 7) Calculation of percent inhibition:
[0000] % inhibition=100−[reading by infrared reader (sample)/reading by infrared reader (blank)]×100
[0072] Partial one-time measurement results for a single concentration are listed in Table 3 (preliminary selection). EC 50 measurement results of representative compounds are listed in Table 4.
[0000]
TABLE 3
Inhibitory activity (percent inhibition) of representative compounds
with concentration of 3 μM against A431 cells EGFR-TK
phosphorylation stimulated by EGF
Inhi-
Inhi-
[nhi-
bition
bition
bition
Percent
Percent
Percent
Compound
(%)
Compound
(%)
Compound
(%)
Example 1
NA
Example 3
85
Example 4
78
Example 5
73
Example 6
24
Example 7
65
Example 8
NA
Example 30
55
Example 31
33
Example 32
87
Example 33
94
Example 34
68
Example 35
23
Example 36
57
Example 37
82
Example 38
94
Example 40
89
Example 41
71
Example 43
91
Example 50
95
Example 51
94
Example 72
97
Example 73
82
Example 105
44
Example 107
52
Example 110
59
Example 118
41
Example 132
64
Example 134
59
Example 141
91
Example 143
96
Example 144
89
Example 150
46
Note:
NA = No activity
[0000]
TABLE 4
Inhibitory activity (EC 50 ) of representative compounds against A431
cells EGFR-TK phosphorylation stimulated by EGF
EC 50
EC 50
EC 50
Compound
(μM)
Compound
(μM)
Compound
(μM)
Example 3
0.15
Example 4
0.58
Example 7
0.4
Example 32
0.09
Example 33
0.038
Example 34
0.76
Example 36
0.98
Example 41
0.30
Example 65
0.23
Example 84
0.013
Example 85
13
Example 110
0.9
Example 141
0.28
Example 143
0.16
[0073] Irreversible Inhibition of Cellular Epidermal Growth Factor Receptor Tyrosine Kinase
(EGFR-TK)
[0074] 1) A431 cells were cultured in a medium prepared by adding 10% FCS into another medium comprising 50% DMEM and 50% F12.
[0075] 2) The A431 cells grown in six-well plates were cultured in a serum-free medium for 24 hours, during the period the medium was replenished once after 12 hours.
[0076] 3) A solution containing a compound to be assessed was added to the A431 cells and cultured for 2 hours, supplemented twice by a medium free of the compound, and then EGF (100 ng/well) was added, and cultured for 5 minutes.
[0077] 4) A431 cell homogenate was prepared by Laemili buffer which comprised 2% sodium dodecyl sulfonate (SDS), 5% 2-mercaptoethanol, 10% glycerol and 5 mM Tris; the pH value is 6.8.
[0078] 5) The A431 cell homogenate was heated for 5 minutes at 100° C.
[0079] 6) Proteins in the A431 cell homogenates were separated by PAGE, transferred onto a nitrocellulose membrane, and an infrared reading was obtained.
[0080] 7) Calculation of percent inhibition:
[0000] % inhibition=100−[reading by infrared reader (medicine)/reading by infrared reader (blank)]×100
[0081] 8) Calculation of percent recovery:
[0000] % recovery=100−% inhibition
[0082] Parts of the results are listed in Table 5.
[0000]
TABLE 5
Activity of representative compounds against A431 cells
EGFR-TK phosphorylation stimulated by EGF
Inhibition
Recovery
Compound
EC 50 (μM)
percent(%)
percent(%)
Activity
Example 32
0.09
78
22
Irreversible inhibitor
Example 33
0.038
89
11
Irreversible inhibitor
Example 84
0.013
14
86
Reversible inhibitor
[0083] Following literature procedured, inhibitory activity of representative compounds against BT474 cells Her-2 receptor TK phosphorylation stimulated by Her-2 was measured, and partial results are listed in Table 6.
[0000]
TABLE 6
Inhibitory activity of representative compounds against BT474 cells
Her-2 receptor TK phosphorylation stimulated by Her-2
EC 50
EC 50
EC 50
Compound
(μM)
Compound
(μM)
Compound
(μM)
Example 43
0.35
Example 72
0.82
Example 73
1.7
Example 105
0.48
Example 108
0.18
Example 150
0.26
[0084] Cell Growth Inhibition Assay (MTS Assay)
[0085] 1. Cell Strain and Reagents
[0086] A431: human epithelial adenocarcinoma cell strain; LoVo: human colorectal cancer cell strain; BT474: breast cancer; SK-Br-3: breast cancer; SIT solution (SIGMA); RPMI1640 culture solution; phosphoric acid buffer; Dimethyl Sulphoxide (DMSO); MTS solution (Promega), 96 well cell culture plate, representative anti-cancer compounds.
[0087] 2. Measurement
[0088] The above-mentioned cells were cultured for several days (RPMI 1640, 10% of bovine serum), collected and suspended in RPMI1640-SIT serum-free medium, placed into a 96-well cell culture plate with each well containing 20,000 cells/100 pt. The cells were cultured overnight under the condition of 5% CO 2 and 37° C. The next day, representative anti-cancer compounds (between 3 and 10 mM) were dissolved by dimethyl sulphoxide (DMSO) as a mother solution. Adriamycin was used as positive control, DMSO was used as negative control. According to experimental design, the mother solution was diluted and added to the 96 well cell culture plate, cultured for 48 hours under the condition of 5% CO 2 and 37° C. Subsequently, 20 μL of MTS solution was added to each well of the 96 well cell culture plate and cultured for another 2 to 4 hours under the condition of 5% CO 2 and 37° C. Absorbance was read at 490 nm wavelength, and converted into cell survival rate.
[0089] Calculation of percent inhibition:
[0000] % inhibition=100−[reading of infrared reader (medicine)/reading of infrared reader (blank)]×100
[0090] For each concentration, there two measurements were taken and the average was obtained. Partial results are listed in Tables 7, 8 and 9.
[0000]
TABLE 7
Growth inhibition activity (EC 50 ) of representative compounds
against A431 cells
EC 50
EC 50
EC 50
Compound
(μM)
Compound
(μM)
Compound
(μM)
Example 3
2
Example 4
1.8
Example 7
5
Example 32
0.6
Example 33
0.10
Example 34
13
Example 36
30
Example 38
0.014
Example 41
1.5
Example 42
0.12
Example 43
0.11
Example 50
0.15
Example 51
0.12
Example 72
0.09
Example 73
0.63
Example 84
0.30
Example 85
35
Example 108
3.0
Example 118
1.9
Example 134
0.9
Example 143
0.25
Example 154
0.11
Tarceva
0.45
Lapatinib
1.19
[0000]
TABLE 8
Growth inhibition activity (EC 50 ) (in μM) of
representative compounds against BT474 and SK-Br-3 cells
Compound
BT474
SK-Br-3
Example 43
0.61
0.52
Example 72
1.31
0.80
Example 73
21.48
2.31
Example 108
1.57
0.53
Lapatinib
0.12
0.07
[0000]
TABLE 9
Growth inhibition activity (EC 50 ) (in μM) of representative
compounds against colorectal cancer LoVo cells
EC 50
EC 50
EC 50
Compound
(μM)
Compound
(μM)
Compound
(μM)
Example 42
3
Example 43
1.5
Example 38
1.6
Example 51
7.6
Example 72
1.8
Example 73
8.0
Example 108
7.0
Example 154
3.1
Adriamycin
1.5
A431 Cell Growth Inhibition Assay (MTT Assay)
Materials and Reagents
[0091] A431, an epidermoid carcinoma cell line; The Cell Bank, Committee on Type Culture Collection Chinese Academy of Science, Shanghai.
[0092] MTT, (Amresco cat.no 0793) 5 mg/mL, dissolved in phosphate buffered saline (PBS), non-sterile. Store at −20° C.
[0093] DMSO, (Analytical reagent) Tianjin Guangfu Fine Chemical Research Institute.
[0094] DMEM, (Gibco, cat.no 12800-058 lot.1272041), Add 2.2 g/L sodium bicarbonate (Sangon, cat.no 0865) and 25 mM HEPEs (Bio.Basic. Inc., cat.no HB0264), then filter the medium with 0.22 μm filter membrane after modulating pH to 7.00. Store at 4° C.
[0095] F12, (Gibco, cat.no 21700-026 lot.268207), Add 2.2 g/L sodium bicarbonate and 25 mM HEPEs, then filter the medium with 0.22 μm filter membrane after modulating pH to 7.00. store at 4° C.
[0096] Trypsin solution, (Invitrogen, cat.no 27250018), 0.25% (w/v), dissolved in phosphate buffered saline (PBS), non-sterile; then add 0.53 mM EDTA after filtering with 0.22 μm filter membrane. Store at 4° C.
[0097] PBS, (pH 7.2˜7.4), NaCl, 8.00 g. KCl, 0.20 g. Na 2 HPO 4 , 1.17 g. KH 2 PO 4 , 0.20 g. Dissolved in 1 L ddH 2 O, autoclaved for sterilization at 121° C. for 20 minutes. Store at 4° C.
[0098] FBS, (similar standard fetal bovine serum, directly use after being thawed out) Lanzhou National Hyclone Bio-Engineering Co., Ltd. lot. 20090521.
Equipment
[0099] 96-well clear flat-bottom cell-culture plates, Corning, cat.no 3599
[0100] Inverted biologic microscope, Model XD-101, Nanjing Jiangnan Novel Optics Co., Ltd.
[0101] CO 2 Incubator, W/C 451 S/N 309493-2488, Thermo-Fisher Scientific Corp.
[0102] Biologic Clean Beach, Model DL-CJ-2N, Harbin Donglian Haer Instrument Manufacturing Co., Ltd.
[0103] Microplate reader, Model 680, Beijing Yuanye Bio Co., Ltd.
[0104] Autoclave, Model YXQG02, Shandong Ande Medical Technology Co., Ltd.
[0105] Plate shaker, Mode MM-I, Shanghai Yarong Biochemistry Instrument Factory.
Procedure
[0106] Cell Complete Growth Medium Preparation
[0107] Mix prepared medium DMEM and F12 in the proportion of 1:1, then add FBS to a final concentration of 10%.
[0108] Compound Preparation
[0109] Dissolved the dried compound sample with 100% DMSO to 2 mM. Then diluted the dissolved compound to 20 μM with cell complete growth medium. For further IC50 determination, made a threefold dilution from 20 μM to 3.04 nM in complete growth medium containing 1% DMSO.
[0110] Cell Preparation
[0111] Prior to the assay, cultured the A431 to logarithmic phase, and then removed medium from cell monolayers and wash the cells once with sterilized PBS. Aspriated the PBS and added 2 mL trypsin solution to cover the cell growth surface, removed 1 mL trypsin solution after soaking about 1 minute. Transferred the cell-culture plate to CO 2 incubator; incubated at 37° C. for 8 minutes to allow cells to dissociate. After the cells detached, added 4 mL complete growth medium containing FBS with pipette to disperse them off and mixed gently to obtain a homogeneous cell suspension. Aspirated some of the cell suspension to a sterilized polypropylene tube, and determined the cell concentration by counting in a hematocytometer chamber under a microscope. Adjusted the cell concentration with growth medium to obtain 2.5×10 4 cells per milliliter.
[0112] Cell Seeding
[0113] Added 100 μL adjusted cell suspension to the 96-well cell-culture plate and occasionally mixed the cell suspension during the seeding process. After seeding cells, incubated the plate at 37° C. overnight with 5% CO 2 in the CO 2 incubator for cell attachment.
[0114] Exposed the Cell to the Compound
[0115] After the cell attachment, added 100 μL prepared compound solutions to the corresponding wells (add PBS to the ambient wells of the plate). The final compound concentrations ranged from 10 μM to 1.52 nM. Incubated the plate at 37° C. with 5% CO 2 for 72 hours in the CO 2 incubator.
[0116] MTT Reaction.
[0117] After the exposure to the compound, removed the cell culture supernatant. Then added 100 μL 0.5 mg/mL MTT solution which dissolved in the growth medium without FBS. Incubated the plate at 37° C. with 5% CO 2 for another 4 hours to allow the MTT reaction to proceed.
[0118] Detection
[0119] After the MTT reaction, discarded the MTT reaction solution. Added 100 μL DMSO to each well, and the plate was agitated on the plate shaker for several minutes to dissolve the formazan. Then, detected the absorbance at 490 nm using microplate reader.
[0000]
TABLE 10
Inhibitory activity (percent inhibition) of representative compounds
with concentration of 3 μM against A431 cells
Inhi-
Inhi-
Inhi-
bition
bition
bition
Percent
Percent
Percent
Compound
(%)
Compound
(%)
Compound
(%)
Example 143
70
Example 145
49
Example 146
52
Example 149
92
Example 150
95
Example 152
95
Example 155
90
Example 156
89
Example 157
85
Example 158
90
Example 159
83
Example 161
49
Example 162
41
Example 163
40
Example 165
53
Example 166
49
Example 167
45
Example 168
41
Example 169
92
Example 170
88
Example 171
86
Example 172
84
Example 173
87
Example 178
88
Example 179
90
Example 180
92
Example 181
94
Example 182
90
Example 183
90
Example 190
91
Example 191
93
Example 192
93
Example 193
90
Example 194
89
[0000]
TABLE 11
Growth inhibition activity (EC 50 ) (in μM) of representative compounds
against A431 cells
Compound
EC 50 (μM)
Compound
EC 50 (μM)
Example 143
1.45
Example 145
3.4
Example 150
0.17
Example 152
0.14
BT-474 Cell Growth Inhibition Assay (SRB Assay)
[0120] Main Materials
[0121] BT-474 human breast cancer cell lines were kindly provided by Dr. Changnian Liu, Pharmaron Beijing Co., Ltd.
[0122] EMEM: purchased from Invitrogen Corporation., catalog number 41500-034, added 2.2 g/l NaHCO3, 25 mM HEPEs, adjusted pH to 7.0, stored at 4° C.
[0123] Similar standard fatal bovine serum (sFBS): purchased from Lanzhou National Hyclone Bio-Engineering Co., Ltd., China.
[0124] Cell culture medium: 90% EMEM and 10% sFBS, stored at 4° C.
[0125] PBS: 8 g/l NaCl, 0.2 g/l KCl, 1.17 g/lNa 2 HPO 4 , 0.2 g/l KH 2 PO 4 , adjusted pH to 7.2-7.4;
[0126] Trypsin/EDTA solution: 0.25% (wt/vol) Trypsin (Invitrogen Corporation, catalog number 27250018) in PBS, added 0.53 mM EDTA, stored at 4° C.;
[0127] 1% (wt/vol) acetic acid.
[0128] SRB: purchased from Sigma-Aldrich, catalog number S9012-5 g; dissolved in 1% acetic acid as a 0.4% (wt/vol) solution, stored at 4° C., protected from light.
[0129] 50% (wt/vol) TCA (Trichloroacetic acid).
[0130] 10 mM unbuffered Tris base solution.
[0131] 96-well cell culture plates: Corning, catalog number 3599.
[0132] 25 cm̂2 cell culture flasks: Corning, catalog number 430168.
[0133] Main Equipment
[0134] Super-clean chamber: Model DL-CJ-2N, Harbin Donglian Haer Instrument Manufacturing Co., Ltd.
[0135] Inverted Microscope: Model XD-101, JiangNanGuangXueYiQiChang, Nanjing, China.
[0136] CO2 incubator: Model 311, Thermo Scientific.
[0137] Autoclave: Model YXQG02, Shandong AnDe Medical Technology Co.,Ltd.
[0138] Micro-plate reader: Model 680, Bio-Rad.
[0139] Automated 96-well plate washer: Model 1575, Bio-Rad.
[0140] Analytical balance: Model BT125D, Sartorius, Max120 g, d=0.01 mg (41 g), 0.1 mg (120 g).
[0141] Plate shaker, Mode MM-I, Shanghai Yarong Biochemistry Instrument Factory
[0142] Methods
[0143] All work was performed under sterile working conditions.
[0144] BT-474 cells were cultured in 37° C., 5% CO2, saturated humidity until logarithmic phase. Discarded culture medium, washed cells once by PBS. Added 1 ml Trypsin/EDTA solution, stood at 37° C. for 5 min, allowed the cells to detach. Added culture medium, adjusted the cells density to 1×10̂5 cells/ml.
[0145] Day 0, added 100 μl/well cells suspension to 96-well cell culture plates. Incubated overnight to let the cells attach completely.
[0146] Day 1, compounds (2 mM in DMSO as stock solution) was diluted to 20 μM in EMEM. Then a fourfold serial dilution was made. These diluted compounds were made as 10× reaction solutions, and the concentration of DMSO was kept at 1%.
[0147] Added 80 μl culture medium and 20 μl 10× compound reaction solution to the testing wells, or vehicle control to the control wells. Co-incubated cells with compounds for another 72 h.
[0148] Day 3, fixed cellular protein by the addition of 100 μl/well of 10% TCA (diluting from 50% TCA) at 4° C. for 1 h. Rinsed TCA using plate washer, and washed five times using distilled water. Removed the residual wash solution with a piece of absorbent paper. Added 100 μl/well 0.4% SRB solution, allowed a 15-30 min staining period. Removed the SRB, and washed the culture plates five times using 1% acetic acid. Removed the residual wash solution with a piece of absorbent paper. Air-dried the culture plates, dissolved the protein-bound dye with 100 μl/well of 10 mM Tris base solution. Shook the plates until the dye was dissolved completely. Measured the OD value by using the micro-plate reader at the wavelength of 570 nm.
[0000] % inhibition ratio=[1−(OD sample −mean OD positive control )/(mean OD positive control −mean OD negative control]×100, where the OD sample was cells growing with compounds, the OD positive control was cells growing with vehicle, OD negative control was blank well with vehicle.
[0000]
TABLE 12
Inhibitory activity (percent inhibition) of representative compounds
with concentration of 3 μM against BT474 cells
Inhi-
Inhi-
Inhi-
bition
bition
bition
Percent
Percent
Percent
Compound
(%)
Compound
(%)
Compound
(%)
Example 143
55
Example 145
80
Example 146
85
Example 149
53
Example 150
56
Example 152
59
Example 155
58
Example 156
60
Example 157
59
Example 158
57
Example 159
53
Example 161
90
Example 162
91
Example 163
87
Example 165
87
Example 166
85
Example 167
84
Example 168
89
Example 169
58
Example 170
56
Example 171
60
Example 172
61
Example 173
44
Example 197
82
Example 198
86
Example 199
87
Example 200
90
Example 201
89
Example 202
92
Example 203
86
Example 206
80
Example 208
83
Example 209
78
Example 211
81
EXAMPLES
Intermediate 1a: Tert-butyl 4-oxopiperidine-1-carboxylate
[0149]
[0150] Hydrated 4-piperidone hydrochloride (8.65 g), BOC 2 O (12.2 g), NaHCO 3 (8.8 g), and NaCl (11.2 g) were dissolved in a mixture of tetrahydrofuran (80 mL) and water (80 mL), stirred at room temperature, and allowed to stand overnight for layer separation. The water layer was extracted once with chloroform. The organic phases were combined, washed once with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated to give the title compound as a white solid (11.35 g).
Intermediate 1b: Tert-butyl 3-oxopyrrolidine-1-carboxylate
[0151]
[0152] The title compound was prepared following the procedure for preparation of intermediate 1a except that 3-oxopyrrolidine hydrochloride was substituted for 4-piperidone hydrochloride.
Intermediate 1c: 1-(2-methoxyethyl)piperidin-4-one
[0153]
[0154] Hydrated 4-piperidone hydrochloride (8.65 g), 1-iodo-2-methoxyethane (12.58 g), and K 2 CO 3 (15.55 g) were dissolved in a mixture of tetrahydrofuran (80 mL) and water (80 mL), stirred at room temperature, and allowed to stand overnight for layer separation. The water layer was extracted once with chloroform. The organic phases were combined, washed once with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated in vacuo to give the title compound as an oil.
Intermediate 2a: Tert-butyl 4-((methoxycarbonyl)methylene)piperidine-1-carboxylate
[0155]
[0156] Sodium hydroxide (4.56 g, 0.114 mol) was dissolved in ethanol (210 mL), and trimethyl phosphonoacetate (11.4 g, 0.062 mol) added with stirring. The mixture was stirred for 30 min at room temperature. Tert-butyl 4-oxopiperidine-1-carboxylate (11.35 g, 0.057 mol) was added with stirring at room temperature, and the reaction was allowed to stand overnight. Then, the mixture was acidified with diluted hydrochloric acid until the pH was 4, filtered, concentrated, and partitioned into water and chloroform. Phases were separated. The aqueous phase was extracted once with chloroform. Chloroform phases were combined, washed once with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated in vacuo to give the title compound.
Intermediate 2b: Methyl 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetate
[0157]
[0158] The title compound was prepared following the procedure for the preparation of intermediate 2a except that 1-(2-methoxyethyl)piperidin-4-one was substituted for 4-oxopiperidine-1-carboxylate.
Intermediate 2c: (E/Z)-tert-butyl 3-((methoxycarbonyl)methylene)pyrrolidine-1-carboxylate
[0159]
[0160] The title compound was prepared following the procedure for the preparation of intermediate 2a except that tert-butyl 3-oxopyrrolidine-1-carboxylate was substituted for 4-oxopiperidine-1-carboxylate.
Intermediate 3a: 2-(1-(tert-butoxycarbonyl)piperidin-4-ylidene)acetic Acid
[0161]
[0162] The above obtained tert-butyl 4-((methoxycarbonyl)methylene)piperidine-1-carboxylate was dissolved in a mixture of tetrahydrofuran (60 mL) and methanol (60 mL). 1N lithium hydroxide (60 mL) was added with stirring at room temperature, and the reaction mixture was allowed to stand overnight. Then, the mixture was extracted three times with dichloromethane. The organic phase was separated. The aqueous phase was acidified with 1N hydrochloric acid until the pH value was about 4 and extracted three times with dichloromethane. The organic phases were combined, washed once with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated in vacuo to give the title compound.
Intermediate 3b: 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetic Acid.
[0163]
[0164] The title compound was prepared following the procedure for the preparation of intermediate 3a except that methyl 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetate was substituted for tert-butyl 4-((methoxycarbonyl)methylene)piperidine-1-carboxylate.
Intermediate 3c: (E/Z)-2-(1-(tert-butoxycarbonyl)pyrrolidin-3-ylidene)acetic Acid
[0165]
[0166] The title compound was prepared following the procedure for the preparation of the intermediate 3a except that (E/Z)-tert-butyl 3-((methoxycarbonyl)methylene)pyrrolidine-1-carboxylate was substituted for tert-butyl 4-((methoxycarbonyl)methylene)piperidine-1-carboxylate.
Intermediate 4a: N 4 -(3-ethynylphenyl)quinazoline-4,6-diamine
[0167]
[0168] 2 g of iron powder was immersed in diluted hydrochloric acid for 30 min, filtered, and washed with water. The washed iron powder, 0.1 g of N-(3-ethynylphenyl)-6-nitroquinazolin-4-amine, 25 mL of ethanol-water solution (water:ethanol=1:2), and 0.3 mL of acetic acid were added into a four-neck flask, and refluxed for one hour with mechanical stirring. After reaction completion, the mixture was cooled to room temperature, filtered, concentrated and ethyl acetate was added. The mixture was washed three times with hydrochloric acid. The aqueous layer was combined and made alkaline with Na 2 CO 3 until the pH was about 9. The aqueous layer was extracted three times with ethyl acetate. All organic phases were combined, washed once with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated in vacuo to give the title compound.
[0169] Intermediates 4b-4-r were prepared following the procedure for the preparation of intermediate 4a.
Intermediate 4b: N 4 -(4-(benzyloxy)-3-chlorophenyl)quinazoline-4,6-diamine
[0170]
Intermediate 4c: N 4 -(4-(3-chlorobenzyloxy)-3-chlorophenyl)quinazoline-4,6-diamine
[0171]
Intermediate 4d: N 4 -(4-(3-bromobenzyloxy)-3-chlorophenyl)quinazoline-4,6-diamine
[0172]
Intermediate 4e: N 4 -(4-(3-methoxybenzyloxy)-3-chlorophenyl)quinazoline-4,6-diamine
[0173]
Intermediate 4f: N 4 -(4-(3-ethoxybenzyloxy)-3-chlorophenyl)quinazoline-4,6-diamine
[0174]
Intermediate 4g: N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)quinazoline-4,6-diamine
[0175]
Intermediate 4h: N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-fluoroquinazoline-4,6-diamine
[0176]
Intermediate 41: N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-methoxyquinazoline-4,6-diamine
[0177]
Intermediate 4j: N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-ethoxyquinazoline-4,6-diamine
[0178]
Intermediate 4k: N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-(2-methoxyethoxy)quinazoline-4,6-diamine
[0179]
Intermediate 41: N 4 -(4-(3-chlorobenzyloxy)-3-chlorophenyl)-7-methoxyquinazoline-4,6-diamine
[0180]
Intermediate 4m: N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)-7-methoxyquinazoline-4,6-diamine
[0181]
Intermediate 4n: N 4 -(1-benzyl-1H-indol-5-yl)quinazoline-4,6-diamine
[0182]
Intermediate 4o: N 4 -(1-(3-fluorobenzyl)-1H-indol-5-yl)-7-methoxyquinazoline-4,6-diamine
[0183]
Intermediate 4p: N 4 -(1-benzyl-1H-indol-5-yl)-7-(2-methoxyethoxy)quinazoline-4,6-diamine
[0184]
Intermediate 4q: 7-ethoxy-N 4 -(3-methoxy-4-phenoxyphenyl)quinazoline-4,6-diamine
[0185]
Intermediate 4r: 7-ethoxy-N 4 -(4-(4-fluorophenoxy)-3-methoxyphenyl)quinazoline-4,6-diamine
[0186]
Example 1
Tert-butyl 4-((4-(3-ethynylphenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate
[0187]
[0188] 1 g of 2-(1-(tert-butyloxycarbonyl)piperidine-4-ylidene)acetic acid was added to 20 mL of anhydrous THF in a one-neck flask (100 mL). The solution was stirred and cooled on salt-ice bath. Then, 0.6 mL of isobutyl chloroformate and 0.5 mL of N-methylmorpholine were added, and the reaction mixture was let stir for 20 min 1.046 g of N 4 -(3-ethynylphenyl)quinazoline-4,6-diamine dissolved in 10 mL of pyridine (dried over molecular sieves) and 0.4 mL of N-methylmorpholine were added to the reaction mixture on an ice bath with stirring. After reaction completion, the solvent was evaporated in vacuo and the remaining residue was partitioned with chloroform and water. The chloroform layer was washed once with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a crude product. The crude product was recrystallized from isopropanol. MS (EI) 482 M + .
Example 2
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide trifluoroacetate
[0189]
[0190] Tert-buty-((4-(3-ethynylphenylamino)quinazolin-6-yl-aminocarbonyl)-methylene)piperidine-1-carboxylic ester (92 mg, 0.38 mmol) was dissolved in 10 mL of 20% anhydrous TFA/DCM solution and stirred at room temperature for 2 hours, evaporated in vacuo, and vacuum dried to give the tile compound as a whitish foam. MS: 384 (M+1).
Example 3
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0191]
[0192] N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide trifluoroacetate was dissolved in ethyl acetate. The mixture was washed once with saturated Na 2 CO 3 and once with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give the title product. MS (EI) 384 (M+1).
Example 4
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0193]
[0194] N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide (20 mg, 0.046 mmol), methyl iodide (8.0 mg, 0.056 mmol), anhydrous potassium carbonate (17 mg), and acetonitrile (5 mL) were placed in a one-neck flask (50 mL). The reaction mixture was stirred at room temperature for 24 hours. After reaction completion, the solution was filtered, and evaporated in vacuo to give a solid. The solid was purified by TLC (silica gel plate, thickness 5 mm, chloroform:methanol=95:5). MS: 398 (M+1).
[0195] The compounds of Example 5-8 were prepared following the procedure of Example 4.
Example 5
[0000]
2-(1-Ethylpiperidin-4-ylidene)-N-(4-(3-ethynylphenylamino)quinazolin-6-yl)acetamide. MS: 412 (M+1).
[0000]
Example 6
[0000]
2-(1-benzylpiperidin-4-ylidene)-N-(4-(3-ethynylphenylamino)quinazolin-6-yl)acetamide. MS: 474 (M+1).
[0000]
Example 7
[0000]
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 440 (M−1).
[0000]
Example 8
[0000]
Methyl 2-(4-((4-(3-ethynylphenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidin-1-yl)acetate. MS: 454 (M + ).
[0000]
Example 9
[0000]
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-isopropylpiperidin-4-ylidene)acetamide. MS: 426 (M+1).
[0000]
Example 10
[0000]
N-(4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-(2-hydroxyethyl)piperidin-4-ylidene)acetamide. MS: 428 (M+1).
[0000]
[0202] The compounds of Examples 11-29 were prepared following the procedure of Example 1.
Example 11
[0000]
Tert-butyl 4-((4-(phenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 459 (M + ).
[0000]
Example 12
[0000]
Tert-butyl 4-((4-(3-chloro-4-fluorophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 511 (M + ).
[0000]
Example 13
[0000]
Tert-butyl 4-((4-(3-bromophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 539 (M+1).
[0000]
Example 14
[0000]
Tert-butyl 4-((4-((S)-1-phenylethylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 487 (M + ).
[0000]
Example 15
[0000]
Tert-butyl 4-((4-((R)-1-phenylethylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 487 (M + ).
[0000]
Example 16
[0000]
Tert-butyl 4-((4-(3-chlorophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 493 (M + ).
[0000]
Example 17
[0000]
Tert-butyl 4-((4-(3-chlorophenylamino)-7-fluoroquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 511 (M + ).
[0000]
Example 18
[0000]
Tert-butyl 4-((4-(3-bromophenylamino)-7-methoxyquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 568 (M+1).
[0000]
Example 19
[0000]
Tert-butyl 4-((4-(3-bromophenylamino)-7-ethoxyquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 582 (M+1).
[0000]
Example 20
[0000]
Tert-butyl 4-((7-(2-methoxyethoxy)-4-(3-bromophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 612 (M+1).
[0000]
Example 21
[0000]
Tert-butyl 4-((4-(1H-indol-5-ylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 498 (M + ).
[0000]
Example 22
[0000]
Tert-butyl 4-((4-(3-ethynylphenylamino)-7-methoxyquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 512 (M + ).
[0000]
Example 23
[0000]
Tert-butyl 4-((4-(3-chloro-4-fluorophenylamino)-7-methoxyquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 541 (M + ).
[0000]
Example 24
[0000]
Tert-butyl 4-((4-(1H-indol-5-ylamino)-7-methoxyquinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 528 (M + ).
[0000]
Example 25
[0000]
Tert-butyl 4-((4-(3-bromophenylamino)-7-(3-methoxypropoxy)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 626 (M + ).
[0000]
Example 26
[0000]
Tert-butyl 4-((4-(3-bromophenylamino)-7-(3-morpholinopropoxy)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 681 (M + ).
[0000]
Example 27
[0000]
Tert-butyl 4-((7-(2-methoxyethoxy)-4-(3-ethynylphenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 557 (M+1).
[0000]
Example 28
[0000]
Tert-butyl 4-((7-(2-methoxyethoxy)-4-(3-chloro-4-fluorophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 585 (M + ).
[0000]
Example 29
[0000]
Tert-butyl 4-((4-(1H-indol-5-ylamino)-7-(2-methoxyethoxy)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate. MS: 572 (M + ).
[0000]
[0222] Following the procedure of Examples 2 and 3, the compounds of Examples 30-50 were prepared.
Example 30
[0000]
N-(4-(3-chlorophenylamino)-7-fluoroquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 411 (M+1).
[0000]
Example 31
[0000]
N-(4-(phenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 359 (M+1).
[0000]
Example 32
[0000]
N-(4-(3-chloro-4-fluorophenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 410 (M + ).
[0000]
Example 33
[0000]
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 438 (M + ).
[0000]
Example 34
[0000]
N-(4-((S)-1-phenylethylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide.MS: 387 (M + ).
[0000]
Example 35
[0000]
N-(4-((R)-1-phenylethylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 387 (M + ).
[0000]
Example 36
[0000]
N-(4-(3-chlorophenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 393 (M + ).
[0000]
Example 37
[0000]
N-(4-(3-bromophenylamino)-7-(3-morpholinopropoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 581 (M + ).
[0000]
Example 38
[0000]
N-(4-(3-bromophenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 467 (M + ).
[0000]
Example 39
[0000]
N-(4-(3-bromophenylamino)-7-ethoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 482 (M + ).
[0000]
Example 40
[0000]
N-(4-(3-bromophenylamino)-7-(2-methoxyethoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 512 (M+1).
[0000]
Example 41
[0000]
N-(4-(1H-indol-5-ylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 398 (M+1).
[0000]
Example 42
[0000]
N-(4-(3-ethynylphenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 413 (M + ).
[0000]
Example 43
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 441 (M+1).
[0000]
Example 44
[0000]
N-(4-(1H-indol-5-ylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 428 (M+1).
[0000]
Example 45
[0000]
(S)—N-(7-methoxy-4-(1-phenylethylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 417 (M + ).
[0000]
Example 46
[0000]
(R)—N-(7-methoxy-4-(1-phenylethylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 417 (M + ).
[0000]
Example 47
[0000]
N-(4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 457 (M + ).
[0000]
Example 48
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-7-(2-methoxyethoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 485 (M + ).
[0000]
Example 49
[0000]
N-(4-(3-ethynylphenylamino)-7-(3-morpholinopropoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 526 (M+1).
[0000]
Example 50
[0000]
N-(4-(3-ethynylphenylamino)-7-(3-methoxypropoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 471 (M+1).
[0000]
[0244] Following the procedure of Example 4, the compounds of Examples 51-83 were prepared.
Example 51
[0000]
N-(4-(3-ethynylphenylamino)-7-methoxyquinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 427 (M+1).
[0000]
Example 52
[0000]
N-(7-ethoxy-4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 455 (M + ).
[0000]
Example 53
[0000]
2-(1-ethylpiperidin-4-ylidene)-N-(4-(3-ethynylphenylamino)-7-methoxyquinazolin-6-yl)acetamide. MS: 441 (M + ).
[0000]
Example 54
[0000]
N-(7-ethoxy-4-(3-ethynylphenylamino)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 441 (M + ).
[0000]
Example 55
[0000]
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 452 (M + ).
[0000]
Example 56
[0000]
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 466 (M+1).
[0000]
Example 57
[0000]
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 496 (M+1).
[0000]
Example 58
[0000]
N-(4-(3-bromophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 482 (M+1).
[0000]
Example 59
[0000]
N-(4-(3-bromophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 496 (M+1).
[0000]
Example 60
[0000]
N-(4-(3-bromophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 526 (M + ).
[0000]
Example 61
[0000]
N-(4-(3-bromophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-(3-methoxypropyl)piperidin-4-ylidene)acetamide. MS: 540 (M + ).
[0000]
Example 62
[0000]
N-(4-(3-bromophenylamino)-7-ethoxyquinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 496 (M+1).
[0000]
Example 63
[0000]
N-(4-(3-bromophenylamino)-7-ethoxyquinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 510 (M + ).
[0000]
Example 64
[0000]
N-(4-(3-bromophenylamino)-7-ethoxyquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 540 (M + ).
[0000]
Example 65
[0000]
N-(4-(3-bromophenylamino)-7-(2-methoxyethoxy)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 526 (M + ).
[0000]
Example 66
[0000]
N-(4-(3-bromophenylamino)-7-(3-methoxypropoxy)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 540 (M + ).
[0000]
Example 67
[0000]
N-(4-(3-bromophenylamino)-7-(3-(dimethylamino)propoxy)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 552 (M + ).
[0000]
Example 68
[0000]
N-(4-(3-bromophenylamino)-7-(3-morpholinopropoxy)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 595 (M+1).
[0000]
Example 69
[0000]
N-(4-(3-chlorophenylamino)-7-fluoroquinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 425 (M + ).
[0000]
Example 70
[0000]
N-(4-(3-chlorophenylamino)-7-fluoroquinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 439 (M + ).
[0000]
Example 71
[0000]
N-(4-(3-chlorophenylamino)-7-fluoroquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 469 (M + ).
[0000]
Example 72
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 455 (M + ).
[0000]
Example 73
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-7-methoxyquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide MS: 499 (M + )
[0000]
Example 74
[0000]
N-(4-(3-chloro-4-fluorophenylamino)quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 469 (M + ).
[0000]
Example 75
[0000]
N-(4-(1H-indol-5-ylamino)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 412 (M+1).
[0000]
Example 76
[0000]
N-(4-(1H-indol-5-ylamino)quinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 426 (M+1).
[0000]
Example 77
[0000]
N-(4-(1H-indol-5-ylamino)quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 456 (M + ).
[0000]
Example 78
[0000]
(S)-2-(1-methylpiperidin-4-ylidene)-N-(4-(1-phenylethylamino)quinazolin-6-yl)acetamide. MS: 401 (M + ).
[0000]
Example 79
[0000]
(S)-2-(1-ethylpiperidin-4-ylidene)-N-(4-(1-phenylethylamino)quinazolin-6-yl)acetamide. MS: 415 (M + ).
[0000]
Example 80
[0000]
(S)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)-N-(4-(1-phenylethylamino)quinazolin-6-yl)acetamide. MS: 445 (M + ).
[0000]
Example 81
[0000]
(S)—N-(7-(2-methoxyethoxy)-4-(1-phenylethylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 461 (M + ).
[0000]
Example 82
[0000]
N-(4-(1H-indol-5-ylamino)-7-(2-methoxyethoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 472 (M+1).
[0000]
Example 83
[0000]
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(pyrrolidin-3-ylidene)acetamide. MS: 423 (M+1).
[0000]
Example 84
Comparison Compound A: N-(4-(3-bromophenylamino)quinazolin-6-yl)propionamide
[0278]
[0279] N 4 -(3-bromophenyl)quinazoline-4,6-diamine (100 mg, 0.32 mmol), pyridine (0.3 mL), and DMAP (20 mg) were dissolved in 10 mL of anhydrous THF. The solution was cooled to 5° C. Propionyl chloride (33 mg, 0.35 mmol) was added to the reaction flask dropwise. Ice bath removed was removed, and the reaction mixture was stirred at room temperature and filtered. The filtrate was dried in vacuo to give a yellow solid. The yellow solid was dissolved in ethyl acetate, washed once with saturated Na 2 CO 3 , then with 10% acetic acid, and then with brine. The organic phase was dried, filtered, and stripped of solvent in vacuo to give a crude product which was purified by TLC to give the title compound as a whitish product.
Example 85
Comparison Compound B: N-(4-(3-bromophenylamino)quinazolin-6-yl)acrylamide
[0280]
[0281] The title compound was prepared following the procedure of Example 84 and substituting acryloyl chloride for propionyl chloride.
Example 86
Comparison Compound C: N-(4-(3-bromophenylamino)quinazolin-6-yl)-3-methylbut-2-enamide
[0282]
[0283] The title compound was prepared following the procedure of Example 84 and substituting 3-methyl-butyl-2-en-acyl chloride for propionyl chloride.
Example 87
N-(7-methoxy-4-(2-phenylcyclopropylamino)quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0284]
1) Preparation of 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetyl Chloride Hydrochloride
[0285]
[0286] 2.4 g of 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetic acid was dissolved in 20 mL of thionyl chloride, refluxed for 2 hours, evaporated in vacuo to remove thionyl chloride and give a solid product.
2) Preparation of N-(7-methoxy-4-(2-phenylcyclopropylamino) quinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0287] Following the procedure of Example 84, the title compound was prepared by reacting 2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetyl chloride hydrochloride with N 4 -(7-methoxy-4-(2-phenylcyclopropyl)quinazolin-4,6-diamine
Example 88
N 1 -(4-(3-bromophenylamino)quinazolin-6-yl)-N 4 -(2-(2-(dimethylamino)ethoxy)ethyl)fumaramide
[0288]
[0289] 79 mg of N 4 -(3-bromophenyl)quinazoline-4,6-diamine, 39 mg of maleic anhydride, and 15 mL of THF were placed in a one-neck flask (50 mL) and refluxed. After the reaction was completed, the reaction mixture was evaporated in vacuo and purified by thin layer chromatography.
[0290] The pure product was dissolved in anhydrous THF, and 2-(2-aminoethoxy)ethanol was added. The solution was cooled in ice bath. Subsequently, THF solution containing DCC was added dropwise, ice bath was removed, and the reaction mixture was refluxed for a day. After the reaction was completed, the solution was cooled to room temperature, filtered, and evaporated in vacuo to give crude title product.
[0291] 105 mg of the crude product was dissolved in 20 mL pyridine, and 400 mg of 4-methylbenzene-1-sulfonyl chloride added with stirring at room temperature. After the reaction was completed, the solvent was evaporated in vacuo and the residue was dissolved in ethyl acetate, washed once with saturated Na 2 CO 3 , once with 1N HCl, and once with brine. The organic phase was dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a product.
[0292] The product was dissolved in 10 mL pyridine, and dimethylamine added with stirring at room temparature. After the reaction was completed, the solvent was evaporated in vacuo and the title purified by thin layer chromatography. MS (EI) 528 M + .
Example 89
N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(1-(2-(2-(2-hydroxyethoxy)ethylamino)acetyl)piperidin-4-ylidene)acetamide
[0293]
[0294] 40 mg of N-(4-(3-bromophenylamino)quinazolin-6-yl)-2-(piperidine-4-ylidene)acetamide and 10 ml of THF were added in a one-mouth flask (50 ml), cooled in ice bath, 0.01 mL of 2-chloroacetyl chloride, and 0.02 mL of triethylamine (dried over molecular sieves) were added with stirring at room temperature. After the reaction was completed, the solvent was evaporated in vacuo, the residue was dissolved in ethyl acetate, washed three times with water and once with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a crude product (30 mg).
[0295] The crude product was dissolved in 10 mL of acetonitrile, and 7.3 mg (0.07 mmol) of 2-(2-aminoethoxy)ethanol and 0.02 mL of triethylamine (dried over molecular sieves) were added with stirring at room temperature. After the reaction was completed, the solvent was evaporated in vacuo and the remaining residue was purified by thin layer chromatography. MS (EI) 581 M + .
[0296] Compounds in Examples 90-101 were prepared using literature procedures.
Example 90
N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-(3-morpholinopropoxy)quinazoline-4,6-diamine
[0297]
Example 91
N 4 -(4-(3-fluorobenzyloxy)-3-chlorophenyl)-7-(3-methoxypropoxy)quinazoline-4,6-diamine
[0298]
Example 92
N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)-7-ethoxyquinazoline-4,6-diamine
[0299]
Example 93
N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)-7-methoxyquinazoline-4,6-diamine
[0300]
Example 94
N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)-7-fluoroquinazoline-4,6-diamine
[0301]
Example 95
N 4 -(3-chloro-4-(pyridin-2-ylmethoxy)phenyl)quinazoline-4,6-diamine
[0302]
Example 96
7-methoxy-N 4 -(3-methoxy-4-phenoxyphenyl)quinazoline-4,6-diamine
[0303]
Example 97
7-methoxy-N 4 -(4-(3-methoxyphenoxy)phenyl)quinazoline-4,6-diamine
[0304]
Example 98
N 4 -(2-chloro-4-(pyridin-2-ylmethoxy)phenyl)-7-methoxyquinazoline-4,6-diamine
[0305]
Example 99
N 4 -(4-(benzyloxy)-3-chlorophenyl)-7-methoxyquinazoline-4,6-diamine
[0306]
Example 100
N 4 -(4-(3-chlorobenzyloxy)-3-fluorophenyl)-7-methoxyquinazoline-4,6-diamine
[0307]
Example 101
N 4 -(4-(3-chloro-4-fluorobenzyloxy)phenyl)-7-methoxyquinazoline-4,6-diamine
[0308]
Example 102
Tert-butyl 4-((4-(4-((pyridin-2-yl)methoxy)-3-chlorophenylamino)quinazolin-6-ylcarbamoyl)methylene)piperidine-1-carboxylate
[0309]
[0310] 1 g of 2-(1-(tert-butyloxycarbonyl)piperidine-4-ylidene)acetic acid and 20 mL of anhydrous THF were placed in a one-neck flask (100 mL), dissolved in stirring, and cooled on a salt-ice bath. Then, 0.6 mL of isobutyl chloroformate and 0.5 mL of N-methylmorpholine were added, stirring for 20 mins. Then, 1.046 g of N 4 -(4-3-chloro-(pyridin-2-ylmethoxy)phenyl)quinazoline-4,6-diamine dissolved in 10 mL of pyridine (dried over molecular sieves), and 0.4 mL of N-methylmorpholine were added with stirring to the reaction flask which was previously cooled on an ice bath. After the reaction was completed, the solvent was evaporated in vacuo and the crude product was partitioned with chloroform and water. The chloroform layer was washed once with saturated brine, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give the crude title product which was recrystallized from isopropanol. MS (EI) 601 M + .
Example 103
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide trifluoroacetate
[0311]
Tert-butyl-4-((4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl-aminocarbonyl)-methylene)piperidine-1-carboxylic ester (92 mg, 0.38 mmol) was dissolved in 10 mL of 20% anhydrous TFA/DCM solution with stirring at room temperature for 2 hours, evaporated in vacuo, and vacuum dried to give the title product as a whitish foam solid. MS: 501 (M+1).
Example 104
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0313]
[0314] N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide trifluoroacetate was dissolved in ethyl acetate, washed once with saturated Na 2 CO 3 , and once with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give the title product. MS (EI) 501 (M+1).
[0315] Compounds of Examples 105-115 were prepared following the procedure of Example 104.
Example 105
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 548 (M+1).
[0000]
Example 106
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-7-(3-methoxypropoxy)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 605 (M + ).
[0000]
Example 107
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-ethoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 544 (M + ).
[0000]
Example 108
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 531 (M+1).
[0000]
Example 109
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-fluoroquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 519 (M+1).
[0000]
Example 110
[0000]
N-(7-methoxy-4-(3-methoxy-4-phenoxyphenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 512 (M+1).
[0000]
Example 111
[0000]
N-(7-methoxy-4-(4-(3-methoxyphenoxy)phenylamino)quinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 511 (M + ).
[0000]
Example 112
[0000]
N-(4-(2-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 531 (M+1).
[0000]
Example 113
[0000]
N-(4-(4-(benzyloxy)-3-chlorophenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 531 (M+1).
[0000]
Example 114
[0000]
N-(4-(4-(3-chlorobenzyloxy)-3-fluorophenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 547 (M + ).
[0000]
Example 115
[0000]
N-(4-(4-(3-chloro-4-fluorobenzyloxy)phenylamino)-7-methoxyquinazolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 548 (M+1).
[0000]
Example 116
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0000]
[0328] N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinazolin-6-yl)-2-(1-piperidin-4-ylidene)acetamide (20 mg, 0.046 mmol), methyl iodide (8.0 mg, 0.056 mmol), anhydrous potassium carbonate (17 mg), and acetonitrile (5 mL) were added to a one-neck flask (50 mL), and stirred at room temperature for 24 hours. After the reaction was complete, the solution was filtered, and evaporated in vacuo to give a solid. The solid was purified by TLC (silica gel plate, thickness 5 mm, chloroform:methanol=95:5). MS: 515 (M + ).
[0329] The compounds of Examples 117-118 were prepared following the procedure of Example 116.
Example 117
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-methoxyquinazolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide. MS: 558 (M + ).
[0000]
Example 118
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-methoxyquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 588 (M + ).
[0000]
[0332] The compounds of Examples 119-131 were prepared following literature procedures.
Example 119
6-Amino-4-(3-chlorophenylamino)-7-methoxyquinoline-3-carbonitrile
[0333]
Example 120
6-Amino-4-(3-chloro-4-fluorophenylamino)-7-methoxyquinoline-3-carbonitrile
[0334]
Example 121
6-Amino-4-(3-ethynylphenylamino)-7-methoxyquinoline-3-carbonitrile
[0335]
Example 122
6-Amino-4-(3-bromophenylamino)-7-methoxyquinoline-3-carbonitrile
[0336]
Example 123
6-Amino-4-(3-chloro-4-fluorophenylamino)-7-ethoxyquinoline-3-carbonitrile
[0337]
Example 124
6-Amino-7-ethoxy-4-(3-ethynylphenylamino)quinoline-3-carbonitrile
[0338]
Example 125
6-Amino-4-(3-bromophenylamino)-7-ethoxyquinoline-3-carbonitrile
[0339]
Example 126
6-Amino-4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-methoxyquinoline-3-carbonitrile
[0340]
Example 127
6-Amino-4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-ethoxyquinoline-3-carbonitrile
[0341]
Example 128
4-(4-(3-Fluorobenzyloxy)-3-chlorophenylamino)-6-amino-7-methoxyquinoline-3-carb onitrile
[0342]
Example 129
4-(4-(3-Fluorobenzyloxy)-3-chlorophenylamino)-6-amino-7-ethoxyquinoline-3-carbonitrile
[0343]
Example 130
6-Amino-4-(4-(3-fluorophenoxy)-3-methoxyphenylamino)-7-methoxyquinoline-3-carbonitrile
[0344]
Example 131
6-Amino-7-ethoxy-4-(4-(3-fluorophenoxy)-3-methoxyphenylamino)quinoline-3-carbonitrile
[0345]
Example 132
6-amino-4-(3-chloro-4-fluorophenylamino)quinoline-3-carbonitrile
[0346]
Example 133
6-amino-4-(3-ethynylphenylamino)quinoline-3-carbonitrile
[0347]
Example 134
6-amino-4-(3-bromophenylamino)quinoline-3-carbonitrile
[0348]
Example 135
6-amino-4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)quinoline-3-carbonitrile
[0349]
Example 136
4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-6-aminoquinoline-3-carbonitrile
[0350]
Example 137
6-amino-4-(3-chloro-4-fluorophenylamino)-7-(2-methoxyethoxy)quinoline-3-carbonitrile
[0351]
Example 138
6-amino-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinoline-3-carbonitrile
[0352]
Example 139
6-amino-4-(3-bromophenylamino)-7-(2-methoxyethoxy)quinoline-3-carbonitrile
[0353]
Example 140
6-amino-4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-7-(2-methoxyethoxy)quinoline-3-carbonitrile
[0354]
Example 141
4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-6-amino-7-(2-methoxyethoxy)quinoline-3-carbonitrile
[0355]
[0356] The compounds of Examples 142-155 were prepared following the procedure of Example 104.
Example 142
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 554 (M+1).
[0000]
Example 143
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 568 (M+1).
[0000]
Example 144
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 571 (M + ).
[0000]
Example 145
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 586 (M+1).
[0000]
Example 146
[0000]
N-(4-(3-chloro-4-(3-fluorophenoxy)phenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 558 (M+1).
[0000]
Example 147
[0000]
N-(4-(3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 461 (M + ).
[0000]
Example 148
[0000]
N-(4-(3-chlorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 448 (M+1).
[0000]
Example 149
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 510 (M+1).
[0000]
Example 150
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 480 (M+1).
[0000]
Example 151
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 466 (M+1).
[0000]
Example 152
[0000]
N-(3-cyano-7-ethoxy-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 452 (M+1).
[0000]
Example 153
[0000]
N-(3-cyano-4-(3-ethynylphenylamino)-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 438 (M+1).
[0000]
Example 154
[0000]
N-(4-(3-bromophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 506 (M + ).
[0000]
Example 155
[0000]
N-(4-(3-bromophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide. MS: 493 (M+1).
[0000]
[0371] The compounds of Examples 156-164 were prepared following the procedure of Example 116.
Example 156
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 494 (M+1).
[0000]
Example 157
[0000]
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 537 (M + ).
[0000]
Example 158
[0000]
N-(3-cyano-7-ethoxy-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 466 (M+1).
[0000]
Example 159
[0000]
N-(3-cyano-7-ethoxy-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 510 (M+1).
[0000]
Example 160
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 582 (M+1).
[0000]
Example 161
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 626 (M+1).
[0000]
Example 162
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide. MS: 600 (M+1).
[0000]
Example 163
[0000]
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 643 (M + ).
[0000]
Example 164
[0000]
N-(4-(3-ethynylphenylamino)-7-methoxyquinazolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide. MS: 471 (M + ).
[0000]
[0381] The compounds of Examples 165-173 were prepared following the procedure of Example 104.
Example 165
[0000]
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-(2-methoxyetho xy)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0000]
[0383] MS: 599 (M+1)
Example 166
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyanoquinolin-6-yl)-2-(ppiperidin-4-ylidene)acetamide
[0384]
[0385] MS:525 (M+1)
Example 167
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0386]
[0387] MS:616 (M+1)
Example 168
[0388] N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyanoquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0000]
[0389] MS:542 (M+1)
Example 169
N-(3-cyano-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0390]
[0391] MS:482 (M+1)
Example 170
N-(3-cyano-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0392]
[0393] MS:408 (M+1)
Example 171
N-(4-(3-bromophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0394]
[0395] MS:536 (M+1)
Example 172
N-(4-(3-bromophenylamino)-3-cyanoquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0396]
[0397] MS:462 (M+1)
Example 173
N-(4-(3-chloro-4-fluorophenylamino)-3-cyanoquinolin-6-yl)-2-(piperidin-4-ylidene)acetamide
[0398]
[0399] MS:436 (M+1)
[0400] The compounds of Examples 174-211 were prepared following the procedure of Example 116.
Example 174
N-(4-(3-chloro-4-fluorophenylamino)-3-cyanoquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0401]
[0402] MS:450 (M+1)
Example 175
N-(4-(3-chloro-4-fluorophenylamino)-3-cyanoquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0403]
[0404] MS:494 (M+1)
Example 176
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0405]
[0406] MS:480 (M+1)
Example 177
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0407]
[0408] MS:524 (M+1)
Example 178
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0409]
[0410] MS:508 (M+1)
Example 179
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-proplpiperidin-4-ylidene)acetamide
[0411]
[0412] MS:522 (M+1)
Example 180
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0413]
[0414] MS:524 (M+1)
Example 181
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0415]
[0416] MS:538 (M+1)
Example 182
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0417]
[0418] MS:552 (M+1)
Example 183
N-(4-(3-chloro-4-fluorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0419]
[0420] MS:568 (M+1)
Example 184
N-(3-cyano-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0421]
[0422] MS:422 (M+1)
Example 185
N-(3-cyano-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0423]
[0424] MS:466 (M+1)
Example 186
N-(3-cyano-4-(3-ethynylphenylamino)-7-methoxyquinolin-6-yl)-2-(1-(2-methoxy ethyl)piperidin-4-ylidene)acetamide
[0425]
[0426] MS:496 (M+1)
Example 187
N-(3-cyano-4-(3-ethynylphenylamino)-7-methoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0427]
[0428] MS:452 (M+1)
Example 188
N-(3-cyano-7-ethoxy-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0429]
[0430] MS:480 (M+1)
Example 189
N-(3-cyano-7-ethoxy-4-(3-ethynylphenylamino)quinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0431]
[0432] MS:494 (M+1)
Example 190
N-(3-cyano-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0433]
[0434] MS:496 (M+1)
Example 191
N-(3-cyano-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0435]
[0436] MS:510 (M+1)
Example 192
N-(3-cyano-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0437]
[0438] MS:524 (M+1)
Example 193
N-(3-cyano-4-(3-ethynylphenylamino)-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0439]
[0440] MS:540 (M+1)
Example 194
N-(4-(3-bromophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-m ethylpiperidin-4-ylidene)acetamide
[0441]
[0442] MS:550 (M+1)
Example 195
N-(4-(3-bromophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0443]
[0444] MS:520 (M+1)
Example 196
N-(4-(3-bromophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0445]
[0446] MS:594 (M+1)
Example 197
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0447]
[0448] MS:569 (M+1)
Example 198
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0449]
[0450] MS:613 (M+1)
Example 199
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0451]
[0452] MS:597 (M+1)
Example 200
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0453]
[0454] MS:613 (M+1)
Example 201
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0455]
[0456] MS:627 (M+1)
Example 202
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0457]
[0458] MS:641 (M+1)
Example 203
N-(4-(3-chloro-4-(pyridin-2-ylmethoxy)phenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0459]
[0460] MS:657 (M+1)
Example 204
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0461]
[0462] MS: 586 (M+1)
Example 205
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-methoxyquinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0463]
[0464] MS: 630 (M+1)
Example 206
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0465]
[0466] MS: 614 (M+1)
Example 207
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-ethoxyquinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0467]
[0468] MS:628 (M+1)
Example 208
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-methylpiperidin-4-ylidene)acetamide
[0469]
[0470] MS:630 (M+1)
Example 209
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-ethylpiperidin-4-ylidene)acetamide
[0471]
[0472] MS:644 (M+1)
Example 210
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-propylpiperidin-4-ylidene)acetamide
[0473]
[0474] MS:658 (M+1)
Example 211
N-(4-(4-(3-fluorobenzyloxy)-3-chlorophenylamino)-3-cyano-7-(2-methoxyethoxy)quinolin-6-yl)-2-(1-(2-methoxyethyl)piperidin-4-ylidene)acetamide
[0475]
[0476] MS:674 (M+1)
[0477] While particular embodiments of the invention have been shown and described, it will be obvious to those skilled in the art that changes and modifications may be made without departing from the invention in its broader aspects, and therefore, the aim in the appended claims is to cover all such changes and modifications as fall within the true spirit and scope of the invention. | A method of preparing a compound of formula (I),
A method for treating cancer or inhibiting growth of cancer cells including administering to a patient mammal in need thereof a pharmaceutical preparation including the compound. A method of treating or preventing a physiological disorder caused by abnormal protein tyrosine kinase activity in a mammal including administering to a mammal a pharmaceutical preparation including the compound. | 2 |
FIELD
[0001] The invention relates generally to a multiple speed transmission having a plurality of planetary gear sets and a plurality of torque transmitting devices, and more particularly to a transmission having eight or more speeds, four planetary gear sets and a plurality of torque transmitting devices.
BACKGROUND
[0002] The statements in this section merely provide background information related to the present disclosure and may or may not constitute prior art.
[0003] A typical multiple speed transmission uses a combination of friction clutches or brakes, planetary gear arrangements and fixed interconnections to achieve a plurality of gear ratios. The number and physical arrangement of the planetary gear sets, generally, are dictated by packaging, cost and desired speed ratios.
[0004] While current transmissions achieve their intended purpose, the need for new and improved transmission configurations which exhibit improved performance, especially from the standpoints of efficiency, responsiveness and smoothness and improved packaging, primarily reduced size and weight, is essentially constant. Accordingly, there is a need for an improved, cost-effective, compact multiple speed transmission.
SUMMARY
[0005] A transmission is provided having an input member, an output member, four planetary gear sets, a plurality of coupling members and a plurality of torque transmitting devices. Each of the planetary gear sets includes first, second and third members. The torque transmitting devices are for example clutches and brakes.
[0006] In an embodiment of the present invention, a transmission is provided having an input member, an output member, a first, second, third and fourth planetary gear sets each having sun gears, carrier members and ring gears.
[0007] In another embodiment of the present invention, the input member is continuously interconnected with the sun gear of the first planetary gear set.
[0008] In yet another embodiment of the present invention, the output member is continuously interconnected with the carrier member of the fourth planetary gear set.
[0009] Additionally, in another embodiment of the present invention, a first interconnecting member continuously interconnects the carrier member of the first planetary gear set with the ring gear of the second planetary gear set.
[0010] In yet another embodiment of the present invention, a second interconnecting member continuously interconnects the sun gear of the second planetary gear set with the sun gear of the third planetary gear set
[0011] In yet another embodiment of the present invention, a third interconnecting member continuously interconnects the carrier member of the second planetary gear set with the ring gear of the third planetary gear set.
[0012] In yet another embodiment of the present invention, a fourth interconnecting member continuously interconnects the carrier member of the third planetary gear set with the ring gear of the fourth planetary gear set.
[0013] Further, in still another embodiment of the present invention, a first torque transmitting device is selectively engageable to interconnect the input member and the sun gear of the first planetary gear set with the sun gear of the second planetary gear set and the sun gear of the third planetary gear set.
[0014] In still another embodiment of the present invention, a second torque transmitting device is selectively engageable to interconnect the input member and the sun gear of the first planetary gear set with the carrier member of the second planetary gear set and the ring gear of the third planetary gear set.
[0015] In still another embodiment of the present invention, a third torque transmitting device is selectively engageable to interconnect the carrier member of the third planetary gear set with the ring gear of the fourth planetary gear set.
[0016] In still another embodiment of the present invention, a fourth torque transmitting device is selectively engageable to interconnect the ring gear of the first planetary gear set with the stationary member.
[0017] In still another embodiment of the present invention, a fifth torque transmitting device is selectively engageable to interconnect the carrier member of the first planetary gear set and the ring gear of the second planetary gear set with the stationary member.
[0018] In still another embodiment of the present invention, a sixth torque transmitting device is selectively engageable to interconnect the carrier member of the second planetary gear set and the ring gear of the third planetary gear set with the stationary member.
[0019] In still another embodiment of the present invention, a seventh torque transmitting device is selectively engageable to interconnect the sun gear of the fourth planetary gear set with the stationary member.
[0020] In still another embodiment of the present invention, the torque transmitting devices are each selectively engageable in combinations of at least three to establish at least eight forward speed ratios and at least one reverse speed ratio between the input member and the output member.
[0021] Further features, aspects and advantages of the present invention will become apparent by reference to the following description and appended drawings wherein like reference numbers refer to the same component, element or feature.
DRAWINGS
[0022] The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way.
[0023] FIG. 1 is a schematic layout of an embodiment of an eight speed transmission according to the present invention; and
[0024] FIG. 2 is a truth table presenting the state of engagement of the various torque transmitting elements in each of the available forward and reverse speeds or gear ratios of the transmission illustrated in FIG. 1 .
DETAILED DESCRIPTION
[0025] The following description is merely exemplary in nature and is not intended to limit the present disclosure, application, or uses.
[0026] Referring now to FIG. 1 , a stick diagram presents a schematic layout of the embodiment of the eight speed transmission 10 according to the present invention. The transmission 10 includes an input shaft or member 12 , a first planetary gear set 14 , a second planetary gear set 16 , a third planetary gear set 18 , a fourth planetary gear set 20 and an output shaft or member 22 .
[0027] The planetary gear set 14 further includes a sun gear member 14 A, a ring gear member 14 C and a planet gear carrier member 14 B that rotatably supports a set of planet gears 14 D (only one of which is shown). The set of planet gears 14 D are each configured to intermesh with both the sun gear member 14 A and the ring gear member 14 C. The sun gear member 14 A is connected for common rotation with an input shaft or member 12 . The ring gear member 14 C is connected for common rotation with a first shaft or interconnecting member 44 . The planet carrier member 14 B is connected for common rotation with a second shaft or interconnecting member 46 .
[0028] The planetary gear set 16 further includes a sun gear member 16 A, a ring gear member 16 C and a planet gear carrier member 16 B that rotatably supports a set of planet gears 16 D (only one of which is shown). The planet gears 16 D are each configured to intermesh with both the sun gear member 16 A and the ring gear member 16 C. The sun gear member 16 A is connected for common rotation with the third shaft or interconnecting member 48 . The ring gear member 16 C is connected for common rotation with the second shaft or interconnecting member 46 . The planet carrier member 16 B is connected for common rotation with a fourth shaft or interconnecting member 50 and with a fifth shaft or interconnecting member 52 .
[0029] The planetary gear set 18 includes a sun gear member 18 A, a ring gear member 18 C and a planet gear carrier member 18 B that rotatably supports a set of planet gears 18 D (only one of which is shown). The set of planet gears 18 D are each configured to intermesh with both the sun gear member 18 A and the ring gear member 18 C. The sun gear member 18 A is connected for common rotation with the third shaft or interconnecting member 48 . The ring gear member 18 C is connected for common rotation with the fifth shaft or interconnecting member 52 . The planet carrier member 18 B is connected for common rotation with a sixth shaft or interconnecting member 54 .
[0030] The planetary gear set 20 includes a sun gear member 20 A, a ring gear member 20 C and a planet gear carrier member 20 B that rotatably supports a set of planet gears 20 D (only one of which is shown). The set of planet gears 20 D are each configured to intermesh with both the sun gear member 20 A and the ring gear member 20 C. The sun gear member 20 A is connected for common rotation with a seventh shaft or interconnecting member 56 . The ring gear member 20 C is connected for common rotation with the sixth shaft or interconnecting member 54 . The planet carrier member 20 B is connected for common rotation with the output shaft or member 22 .
[0031] The input shaft or member 12 is continuously connected to an engine (not shown) or to a turbine of a torque converter (not shown). The output shaft or member 22 is continuously connected with the final drive unit or transfer case (not shown).
[0032] With continued reference to FIG. 1 , transmission 10 further includes torque-transmitting mechanisms or clutches 24 , 26 , 28 and the brakes 30 , 32 , 34 and 36 . Clutches 24 , 26 and 28 are configured to selectively interconnect the shafts or interconnecting members and the members of the planetary gear set, as will be described in detail below. The brakes 30 , 32 , 34 and 36 are configured to selectively interconnect the shafts or interconnecting members and members of the planetary gear sets to a transmission housing 40 , as will be described in detail below. For example, the first clutch 24 is selectively engageable to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The second clutch 26 is selectively engageable to connect the input shaft 12 with the fourth shaft or interconnecting member 50 . The third clutch 28 is selectively engageable to connect the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The first brake 30 is selectively engageable to connect the first shaft or interconnecting member 44 with a stationary element or the transmission housing 40 in order to prevent the first shaft or interconnecting member 44 from rotating relative to the transmission housing 40 . The second brake 32 is selectively engageable to connect the second shaft or interconnecting member 46 with a stationary element or the transmission housing 40 in order to prevent the second shaft or interconnecting member 46 from rotating relative to the transmission housing 40 . The third brake 34 is selectively engageable to connect the fifth shaft or interconnecting member 52 with the stationary element or the transmission housing 40 in order to prevent the fifth shaft or interconnecting member 52 from rotating relative to the transmission housing 40 . The fourth brake 36 is selectively engageable to connect the seventh shaft or interconnecting member 56 with the stationary element or the transmission housing 40 in order to prevent the seventh shaft or interconnecting member 56 from rotating relative to the transmission housing 40 .
[0033] Referring now to FIGS. 1 and 2 , the operation of the embodiment of the eight speed transmission 10 will be described. It will be appreciated that the transmission 10 is capable of transmitting torque from the input shaft or member 12 to the output shaft or member 22 in at least eight forward speed or torque ratios and at least one reverse speed or torque ratio with a double overdrive. Each forward and reverse speed or torque ratio is attained by engagement of one or more of the torque-transmitting mechanisms (i.e. first clutch 24 , second clutch 26 , third clutch 28 , first brake 30 , second brake 32 , third brake 34 and fourth brake 36 ), as will be explained below. FIG. 2 is a clutch table presenting the various combinations of torque-transmitting elements that are activated or engaged to achieve the various gear states. Actual numerical gear ratios of the various gear states are also presented although it should be appreciated that these numerical values are exemplary only and that they may be adjusted over significant ranges to accommodate various applications and operational criteria of the transmission 10 . Of course, other gear ratios are achievable depending on the gear diameter, gear teeth count and gear configuration selected.
[0034] For example, to establish reverse gear, the third clutch 28 , the first brake 30 and third brake 34 are engaged or activated. More specifically, the third clutch 28 is engaged to connect the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The first brake 30 connects the first shaft or interconnecting member 44 with the stationary element or the transmission housing 40 in order to prevent the first shaft or interconnecting member 44 from rotating relative to the transmission housing 40 . The third brake 34 connects the fifth shaft or interconnecting member 52 with the stationary element or the transmission housing 40 in order to prevent the fifth shaft or interconnecting member 52 from rotating relative to the transmission housing 40 . Thus, a reverse gear ratio is established between the input member 12 and the output member 22 .
[0035] A first gear is established by engaging or activating the first clutch 24 , the third brake 34 and fourth brake 36 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The third brake 34 connects the fifth shaft or interconnecting member 52 with the stationary element or the transmission housing 40 in order to prevent the fifth shaft or interconnecting member 52 from rotating relative to the transmission housing 40 . The fourth brake 36 connects the seventh shaft or interconnecting member 56 with the stationary element or the transmission housing 40 in order to prevent the seventh shaft or interconnecting member 56 from rotating relative to the transmission housing 40 . Thus, a first gear ratio is established between the input member 12 and the output member 22 .
[0036] A second gear is established by engaging or activating, the first clutch 24 , the third clutch 28 and third brake 34 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The third brake 34 connects the fifth shaft or interconnecting member 52 with the stationary element or the transmission housing 40 in order to prevent the fifth shaft or interconnecting member 52 from rotating relative to the transmission housing 40 . Thus, a second gear ratio is established between the input member 12 and the output member 22 .
[0037] A third gear is established by engaging or activating the first clutch 24 , the second brake 32 and fourth brake 36 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The second brake 32 connects the second shaft or interconnecting member 46 with a stationary element or the transmission housing 40 in order to prevent the second shaft or interconnecting member 46 from rotating relative to the transmission housing 40 . The fourth brake 36 connects the seventh shaft or interconnecting member 56 with the stationary element or the transmission housing 40 in order to prevent the seventh shaft or interconnecting member 56 from rotating relative to the transmission housing 40 . Thus, a third gear ratio is established between the input member 12 and the output member 22 .
[0038] A fourth gear is established by engaging or activating the first clutch 24 , the third clutch 28 and second brake 32 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The second brake 32 connects the second shaft or interconnecting member 46 with a stationary element or the transmission housing 40 in order to prevent the second shaft or interconnecting member 46 from rotating relative to the transmission housing 40 . Thus, a fourth gear ratio is established between the input member 12 and the output member 22 .
[0039] A fifth gear is established by engaging or activating the first clutch 24 , the third clutch 28 and first brake 30 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The first brake 30 connects the first shaft or interconnecting member 44 with the stationary element or the transmission housing 40 in order to prevent the first shaft or interconnecting member 44 from rotating relative to the transmission housing 40 . Thus, a fifth gear ratio is established between the input member 12 and the output member 22 .
[0040] A sixth gear is established by engaging or activating the first clutch 24 , the second clutch 26 and the third clutch 28 . More specifically, the first clutch 24 is engaged to connect the input shaft or member 12 with the third shaft or interconnecting member 48 . The second clutch 26 connects the input shaft 12 with the fourth shaft or interconnecting member 50 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . Thus, a sixth gear ratio is established between the input member 12 and the output member 22 .
[0041] A seventh gear is established by engaging or activating the second clutch 26 , the third clutch 28 and first brake 30 . More specifically, the second clutch 26 connects the input shaft 12 with the fourth shaft or interconnecting member 50 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The first brake 30 connects the first shaft or interconnecting member 44 with the stationary element or the transmission housing 40 in order to prevent the first shaft or interconnecting member 44 from rotating relative to the transmission housing 40 . Thus, a seventh gear ratio is established between the input member 12 and the output member 22 .
[0042] An eighth gear is established by engaging or activating the second clutch 26 , the third clutch 28 and second brake 32 . More specifically, the second clutch 26 connects the input shaft 12 with the fourth shaft or interconnecting member 50 . The third clutch 28 connects the sixth shaft or interconnecting member 54 with the seventh shaft or interconnecting member 56 . The second brake 32 connects the second shaft or interconnecting member 46 with a stationary element or the transmission housing 40 in order to prevent the second shaft or interconnecting member 46 from rotating relative to the transmission housing 40 . Thus, an eighth gear ratio is established between the input member 12 and the output member 22 .
[0043] It will be appreciated that the foregoing explanation of operation and gear states of the eight speed transmission 10 assumes, first of all, that all the clutches and brakes not specifically referenced in a given gear state are inactive or disengaged and, second of all, that during gear shifts, i.e., changes of gear state, between at least adjacent gear states, a clutch or brake engaged or activated in both gear states will remain engaged or activated.
[0044] The description of the invention is merely exemplary in nature and variations that do not depart from the gist of the invention are intended to be within the scope of the invention. For example, the present invention contemplates that multiple components, i.e. members of the planetary gear sets, maybe formed integrally with an interconnecting member or shaft to form a single member which may be rotatable or fixed. Moreover, two or more shafts or interconnecting members may be joined to form a single member or shaft. Additionally, the present invention contemplates several alternatives to increase the number of ranges and ratio spreads of the transmission 10 . More specifically, the clutched, input and output planetary components may be changed to add overdrive ranges instead of under drive ranges. The planetary gear set 20 and clutch 28 may be housed in a separate housing from a housing that houses planetary gear sets 14 , 16 and 18 . Alternatively, planetary gear set 20 and clutch 28 may be housed in an AWD/4WD transfer case to conserve space. Such variations are not to be regarded as a departure from the spirit and scope of the invention. | A transmission of the present invention has an input member, an output member, four planetary gear sets, a plurality of coupling members and a plurality of torque transmitting devices. Each of the planetary gear sets includes a sun gear, a carrier member supporting a plurality of planet pinion gears and a ring gear member. The torque transmitting devices may include clutches and brakes. The torque transmitting devices are selectively engageable in combinations of at least three to establish a plurality forward speed ratios and at least one reverse speed ratio. | 5 |
BACKGROUND
Many subterranean formations contain hydrocarbon based fluids, e.g. oil or gas, that can be produced to a surface location for collection. Generally, a wellbore is drilled, and a completion is moved downhole to facilitate production of desired fluids from the surrounding formation. In many applications, the wellbore completion includes one or more well tools, such as packers, valves or other tools useful in a given application, that are selectively actuated once the completion is deployed in the wellbore.
Actuation of many well devices is accomplished by physically moving a mechanical actuating member that changes the tool from one state to another. Examples include moving a valve from a closed position to an open position, setting a packer, or actuating a wide variety of other well tool types. The force to actuate such well tools can be provided by, for example, hydraulic pressure, solenoid actuators or combinations of electric motors, gear boxes and ball screw actuators.
Actuation of a well device typically occurs during movement of the completion downhole or after the completion has been fully deployed at the downhole location. Often, the downhole environment in which such tools are operated is a relatively harsh environment, susceptible to relatively high temperatures, pressures and deleterious substances. Accordingly, actuators having a high degree of complexity in construction or operation can have an increased susceptibility to malfunction due to the adverse conditions.
SUMMARY
In general, the present invention provides a system and method for dependable actuation of well devices, e.g. well tools, used in a wellbore environment. An actuator is positioned to move or actuate a specific downhole device from one state to another by physical movement of an actuator member of the downhole device. The actuator utilizes a phase change material to provide the motive force to move the actuator member. Upon providing an appropriate input, the phase change material can be caused to undergo a selective phase change, thus providing power for actuation of the well device.
BRIEF DESCRIPTION OF THE DRAWINGS
Certain embodiments of the invention will hereafter be described with reference to the accompanying drawings, wherein like reference numerals denote like elements, and:
FIG. 1 is a front elevation view of a completion deployed in wellbore, according to an embodiment of the present invention;
FIG. 2 is a schematic illustration of an actuator system coupled to a downhole well device for actuation of the well device, according to an embodiment of the present invention;
FIG. 3 is a schematic illustration of another embodiment of the actuator system illustrated in FIG. 2 ;
FIG. 4 is a graphical representation of pressure that can be applied by a phase change material utilized with the actuator system illustrated in FIG. 3 ;
FIG. 5 is a schematic illustration of another embodiment of the actuator system illustrated in FIG. 2 ;
FIG. 6 is a schematic illustration of another embodiment of the actuator system illustrated in FIG. 2 , showing a valve in a closed position; and
FIG. 7 is a schematic illustration similar to that of FIG. 6 , but showing the valve in an open position.
DETAILED DESCRIPTION
In the following description, numerous details are set forth to provide an understanding of the present invention. However, it will be understood by those of ordinary skill in the art that the present invention may be practiced without these details and that numerous variations or modifications from the described embodiments may be possible.
The present invention relates to well systems comprising one or more wellbore completions having devices that are mechanically actuated from one state of operation to another. Generally, a completion is deployed within a wellbore drilled in a formation containing desirable production fluids. The completion may be used, for example, in the production of hydrocarbon based fluids, e.g. oil or gas, in well treatment applications or in other well related applications. In many applications, the wellbore completion incorporates a plurality of devices, e.g. well tools, that may be individually actuated at desired times.
Referring generally to FIG. 1 , a well system 20 is illustrated as comprising a completion 22 deployed for use in a well 24 having a wellbore 26 that may be lined with a wellbore casing 28 . Completion 22 extends downwardly from a wellhead 30 disposed at a surface location 32 , such as the surface of the Earth or a seabed floor. Wellbore 26 is formed, e.g. drilled, in a formation 34 that may contain, for example, desirable fluids, such as oil or gas. Completion 22 is located within the interior of casing 28 and comprises a tubing 36 and at least one device 38 , e.g. well tool, mechanically actuated by a corresponding actuator 40 . By way of example, completion 22 may comprise two devices 38 , as illustrated. However, a variety of numbers and types of mechanically actuated devices 38 can be used in the completion, depending on the overall design of well system 20 .
In the embodiment illustrated, actuators 40 are phase change actuators able to apply directed forces upon undergoing a phase change, such as a transition from a solid state to a liquid state. Upon appropriate input to each actuator 40 , the phase change is initiated and a change in volume of a given phase change material occurs. This volumetric change, e.g. a volumetric expansion as the material transitions from a solid to a liquid, can be used to physically move components which, in turn, actuate the corresponding wellbore device 38 . The volumetric change can be initiated by, for example, an electrical input provided to each actuator by an appropriate electrical line or lines 42 . The ability to provide signals to each actuator enables the well operator to selectively actuate each individual device 38 when desired.
Referring now to FIG. 2 , an embodiment of a phase change actuator 40 is illustrated as positioned in a wellbore device 38 . In this embodiment, a phase change material 44 is deployed in a chamber or cavity 46 and trapped within the cavity 46 by a movable component 48 . Movable component 48 may comprise a dynamic seal, such as a piston 50 having one or more sealing rings 52 . In this embodiment, piston 50 is deployed within a cylinder 54 along which the piston moves when phase change material 44 undergoes a phase change. For example, the phase change material 44 may undergo volumetric expansion as it transitions from a solid state to liquid state. This transition from a solid to liquid state can be initiated by a thermal unit 56 powered by electricity supplied via electrical line 42 . In the embodiment illustrated, thermal unit 56 comprises an electrical heater element 58 for selectively heating phase change material 44 to cause the phase change from solid state to liquid state. However, thermal unit 56 also may comprise an electric cooling element 60 , such as a thermo-electric cooling (TEC) unit, for selectively cooling phase change material 44 and thus causing a reverse transition, e.g. from liquid state to solid state. Additionally, chamber 46 may be insulated to facilitate the heating and/or cooling of phase change material 44 .
Movable component 48 is coupled to an actuating member 62 of wellbore device 38 by an appropriate linking element 64 . Accordingly, when phase change material 44 undergoes volumetric expansion due to phase change, movable component 48 is forced along cylinder 54 . The movement of component 48 forces the movement of actuating member 62 , via linkage 64 , for mechanical actuation of wellbore device 38 . By way of example, wellbore device 38 may comprise a packer actuated, at least in part, by physical movement of actuating member 62 . In another embodiment, wellbore device 38 may comprise a valve actuated, at least in part, by physical movement of valve actuating member 62 .
In this embodiment, actuator 40 operates the wellbore device 38 , e.g. a valve, a packer or another well device, when power is connected or disconnected from thermal unit 56 . Insulation of chamber 46 enables the use of a relatively small amount of electrical power to be transmitted downhole to thermal unit 56 to melt or solidify phase change material 44 . Alternatively, the electrical power can be generated downhole by, for example, a battery coupled to thermal unit 56 . When the electrical power is supplied to thermal unit 56 , phase change material 44 undergoes a change in volume which changes the pressure acting against movable component 48 , e.g. dynamic piston 50 . If the pressure opposing movement of piston 50 is less than the pressure applied by phase change material 44 , the piston moves and performs useful work, such as actuating wellbore device 38 .
The phase change material 44 may be selected such that the actuating forces are derived by a phase change from solid state to liquid state or vice versa. However, in other applications, phase change material 44 may be selected to exert the requisite forces during changes between gas, liquid and/or solid states. In the embodiment described, the actuating work can be accomplished by a phase change material formed of a polymer material, however other types of phase change materials can be utilized.
A specific example of a well device 38 is illustrated in FIG. 3 . In this embodiment, well device 38 comprises a flow control valve 66 having a generally tubular outer housing 68 with radial ports 70 formed therethrough. Flow control valve 66 further includes an internal flow passage 72 that may be selectively placed in communication with ports 74 to enable flow of fluid through ports 70 and internal flow passage 72 . This flow, however, is controlled by an adjustable choke 74 slidingly mounted within outer housing 68 for engagement with a sealing surface 76 . When adjustable choke 74 is sealed against sealing surface 76 , fluid does not flow between ports 70 and internal flow passage 72 . However, upon displacement of adjustable choke 74 from sealing surface 76 , fluid flow is enabled.
The adjustable choke 74 is actuated by movable component 48 , e.g. a piston, that forms a dynamic seal via a seal ring 78 . Chamber 46 is disposed at an opposite end of movable member 48 from adjustable choke 74 and is filled with volumetric phase change material 44 . Thermal unit 56 is deployed within outer housing 68 adjacent cavity 46 to selectively heat and/or cool phase change material 44 . Electrical power is supplied to thermal unit 56 via an electrical input 80 . In this embodiment, an insulating material 82 surrounds chamber 46 and may be deployed either along the exterior of tubular outer housing 68 or within the outer housing. Additionally, a position sensor 84 may be deployed along movable component 48 to determine the position of component 48 and thus the position of adjustable choke 74 and the degree to which fluid flow is enabled. Position sensor 84 can be used to output a position signal, thereby creating a closed loop system able to provide feedback as to the actuation of device 38 relative to the electrical power input to thermal unit 56 .
In many operating conditions, e.g. in gas production wells, an advantage of phase change actuator 40 is that the differential pressure across a dynamic seal is less than the absolute pressure applied upstream of the valve, as illustrated in FIG. 4 . FIG. 4 simply provides one graphical example of upstream pressure relative to choke diameter and the differential pressure across the dynamic seal of such a valve with a given amount of back pressure. By properly defining the operational specifications of actuator 40 , the pressure ratings of the phase change actuator can be relatively high.
Another example of valve 66 is illustrated in FIG. 5 . This valve embodiment can be used in high-temperature gas lift applications where the geothermal temperature exceeds the melting point of phase change material 44 . An annular volume of the phase change material 44 is confined between dynamic seals 86 and 88 which have different diameters. A choke 90 is positioned by regulating the temperature of phase change material 44 between dynamic seals 86 and 88 via thermal unit 56 . For example, choke 90 can be positioned in sealing engagement with a flow control seal surface 91 by initiating a phase change to increase the volume of phase change material 44 , thereby completely blocking fluid flow through ports 70 . By then decreasing the volume of phase change material 44 , via thermal unit 56 , choke 90 can be moved away from flow control seal surface 91 to enable gas flow through valve 66 . In the embodiment illustrated, a thermal insulator 92 is deployed along an exterior surface of tubular outer housing 68 . Some heat transfer, however, is allowed between the inner surface of a venturi 94 and the sealed chamber 46 . The cooling effect of throttling gases through valve 66 is utilized to decrease the power required to electrically cool the phase change material via, for example, a TEC contained in thermal unit 56 .
Referring to FIGS. 6 and 7 , another embodiment of wellbore device 38 is illustrated in which actuator 40 comprises a puller-type actuator. The actuator uses a movable component 48 in the form of a dynamically sealed movable piston 96 coupled to actuating member 62 by linkage 64 and an indexer 98 . In the specific embodiment illustrated, device 38 is a valve and actuating member 62 comprises a variable choke 100 used to control the flow of fluid between ports 102 and a venturi 104 . The position of variable choke 100 can be set by reciprocating indexer 98 via linkage 64 , as accomplished with conventional indexing mechanisms. The reciprocating movement of linkage 64 and indexer 98 is accomplished by sequential phase changes of the phase change material 44 which is trapped in chamber 46 . Chamber 46 is positioned generally between movable piston 96 and indexer 98 such that piston 96 pulls on linkage 64 and indexer 98 when phase change material 44 undergoes volumetric expansion. Accordingly, the actuating member 62 , e.g. variable choke 100 , can be moved in gradations from a first state, as illustrated in FIG. 6 to a second state, as illustrated in FIG. 7 . In the specific example illustrated, the variable choke 100 is moved between a closed position and a fully open position in increments established by indexer 98 .
With further reference to the embodiment of FIGS. 6 and 7 , chamber 46 is formed by an interior housing 106 disposed within an outer device housing 108 . Outer housing 108 includes an electrical feed-through 110 by which electrical input can be provided to thermal unit 56 to heat and/or cool elements deployed between interior housing 106 and outer housing 108 . The heating and cooling of phase change material 44 creates reciprocating motion of movable piston 96 and the indexing of actuating member 62 to a desired position. In this specific embodiment, the valve further comprises a compensation bellows 112 disposed on an opposite end of movable piston 96 from chamber 46 . The embodiment further comprises a seal bellows 114 deployed between variable choke 100 and indexer 98 . Compensation bellows 112 and seal bellows 114 provide isolation from wellbore fluids and can be filled with a liquid, such as an oil, that is communicated between the seal bellows 114 and the compensation bellows 112 via a liquid flow path 116 . Accordingly, the internal liquid can move from one bellows to the other as the volume of each individual bellows is changed during actuation of the choke.
The examples of wellbore devices illustrated and described herein are just a few examples of the many types of wellbore devices that can be actuated with a phase change actuator. Many other low-power, high work actuator applications are amenable to implementation of phase change actuators. For example, phase change actuators can be used for actuation of a flow tube in a subsurface safety valve, actuation of a flapper valve, actuation of a ball valve, actuation of a variety of packer components, and for actuating many other downhole devices. Additionally, initiation of phase change in the phase change material can be provided by input other than electrical input. In one example, a chemical reaction, e.g. an exothermic chemical reaction, can be initiated to create heat that causes the phase change material 44 to undergo a change of phase sufficient to actuate a given wellbore device 38 .
Accordingly, although only a few embodiments of the present invention have been described in detail above, those of ordinary skill in the art will readily appreciate that many modifications are possible without materially departing from the teachings of this invention. Accordingly, such modifications are intended to be included within the scope of this invention as defined in the claims. | A technique is provided for actuating devices deployed in a wellbore. The technique utilizes an actuator that cooperates with a downhole device, such as a well tool. The actuator has a phase change material that can be caused to undergo a phase change upon an appropriate input. The phase change of the material is used to provide the force necessary for actuation of the downhole device. | 4 |
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation-in-part of copending application Ser. No. 12/488,112, filed Jun. 17, 2009, which claims priority from U.S. Provisional Application No. 61/083,249, filed Jul. 24, 2008 and U.S. Provisional Application No. 61/172,098, filed Apr. 23, 2009, the entireties of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates to high strength, high toughness steel alloys, and in particular, to such an alloy that can be tempered at a significantly higher temperature without significant loss of tensile strength. The invention also relates to a high strength, high toughness, tempered steel article.
[0004] 2. Description of the Related Art
[0005] Age-hardenable martensitic steels that provide a combination of very high strength and fracture toughness are known. Among the known steels are those described in U.S. Pat. No. 4,706,525 and U.S. Pat. No. 5,087,415. The former is known as AF1410 alloy and the latter is sold under the registered trademark AERMET. The combination of very high strength and toughness provided by those alloys is a result of their compositions which include significant amounts of nickel, cobalt, and molybdenum, elements that are typically among the most expensive alloying elements available. Consequently, those steels are sold at a significant premium compared to other alloys that do not contain such elements.
[0006] More recently, a steel alloy has been developed that provides a combination of high strength and high toughness without the need for alloying additions such as cobalt and molybdenum. One such steel is described in U.S. Pat. No. 7,067,019. The steel described in that patent is an air hardening CuNiCr steel that excludes cobalt and molybdenum. In testing, the alloy described in the '019 patent has been shown to provide a tensile strength of about 280 ksi together with a fracture toughness of about 90 ksi √in. The alloy is hardened and tempered to achieve that combination of strength and toughness. The tempering temperature is limited to not more than about 400° F. in order to avoid softening of the alloy and a corresponding loss of strength.
[0007] The alloy described in the '019 patent is not a stainless steel and therefore, it must be plated to resist corrosion. Material specifications for aerospace applications of the alloy require that the alloy be heated at 375° F. for at least 23 hours after being plated in order to remove hydrogen adsorbed during the plating process. Hydrogen must be removed because it leads to embrittlement of the alloy and adversely affects the toughness provided by the alloy. Because this alloy is tempered at 400° F., the 23 hour 375° F. post-plating heat treatment results in over-tempering of parts made from the alloy such that a tensile strength of at least 280 ksi cannot be provided. It would be desirable to have a CuNiCr alloy that can be hardened and tempered to provide a tensile strength of at least 280 ksi and a fracture toughness of about 90 ksi √in, and maintain that combination of strength and toughness when heated at about 375° F. for at least 23 hours, subsequent to being hardened and tempered.
SUMMARY OF THE INVENTION
[0008] The disadvantages of the known alloys as described above are resolved to a large degree by an alloy according to the present invention. In accordance with one aspect of the present invention, there is provided a high strength, high toughness steel alloy that has the following broad and preferred weight percent compositions.
[0000] Element Broad Preferred A Preferred B Preferred C C 0.30-0.55 0.37-0.50 0.30-0.40 0.40-0.47 Mn 0.6-1.3 0.7-0.9 0.8-1.3 0.8-1.3 Si 0.9-2.5 1.3-2.1 1.5-2.5 1.5-2.5 Cr 0.75-2.5 1.2-1.5 1.5-2.5 1.5-2.5 Ni 3.0-7.0 3.7-4.5 3.0-4.5 4.0-5.0 Mo + ½ W 0.4-1.3 0.5-1.1 0.7-0.9 0.7-0.9 Cu 0.5-0.9 0.5-0.6 0.70-0.90 0.70-0.90 Co 0.01 max. 0.01 max. 0.01 max. 0.01 max. V + ( 5/9) × Nb 0.10-1.0 0.2-1.0 0.10-0.25 0.10-0.25 Ti 0.001 max. 0.001 max. 0.005 max. 0.005 max. Al 0.015 max. 0.015 max. Fe Balance Balance Balance Balance
Included in the balance are the usual impurities found in commercial grades of steel alloys produced for similar use and properties. Among said impurities phosphorus is preferably restricted to not more than about 0.01% and sulfur is preferably restricted to not more than about 0.001%. Within the foregoing weight percent ranges, silicon, copper, and vanadium are balanced such that
[0000] 2≦(% Si+% Cu)/(% V+(5/9)×% Nb)≦34.
[0009] The foregoing tabulation is provided as a convenient summary and is not intended to restrict the lower and upper values of the ranges of the individual elements for use in combination with each other, or to restrict the ranges of the elements for use solely in combination with each other. Thus, one or more of the ranges can be used with one or more of the other ranges for the remaining elements. In addition, a minimum or maximum for an element of a broad or preferred composition can be used with the minimum or maximum for the same element in another preferred or intermediate composition. Moreover, the alloy according to the present invention may comprise, consist essentially of, or consist of the constituent elements described above and throughout this application. Here and throughout this specification the term “percent” or the symbol “%” means percent by weight or mass percent, unless otherwise specified.
[0010] In accordance with another aspect of the present invention, there is provided a hardened and tempered steel alloy article that has very high strength and fracture toughness. The article is formed from an alloy having the broad or preferred weight percent composition set forth above. The alloy article according to this aspect of the invention is further characterized by being tempered at a temperature of about 500° F. to 600° F.
DETAILED DESCRIPTION
[0011] The alloy according to the present invention contains at least about 0.30% and preferably at least about 0.32% carbon. Carbon contributes to the high strength and hardness capability provided by the alloy. When higher strength and hardness are desired, the alloy preferably contains at least about 0.40% carbon (e.g., Preferred C). Carbon is also beneficial to the temper resistance of this alloy. Too much carbon adversely affects the toughness provided by the alloy. Therefore, carbon is restricted to not more than about 0.55%, better yet to not more than about 0.50%, and preferably to not more than about 0.47%. The inventor has found that when the alloy contains as little as 0.30% carbon, the upper limit for carbon can be restricted to not more than about 0.40% and the alloy can be balanced with respect to its constituents (e.g., Preferred B) to provide a tensile strength of at least 290 ksi.
[0012] At least about 0.6%, better yet at least about 0.7%, and preferably at least about 0.8% manganese is present in this alloy primarily to deoxidize the alloy. It has been found that manganese also benefits the high strength provided by the alloy. Thus, when higher strength is desired, the alloy contains at least about 1.0% manganese. If too much manganese is present, then an undesirable amount of retained austenite may result during hardening and quenching such that the high strength provided by the alloy is adversely affected. Therefore, the alloy may contain up to about 1.3% manganese. Otherwise, the alloy contains not more than about 1.2% or not more than about 0.9% manganese.
[0013] Silicon benefits the hardenability and temper resistance of this alloy. Therefore, the alloy contains at least about 0.9% silicon and preferably, at least about 1.3% silicon. At least about 1.5% and preferably at least about 1.9% silicon is present in the alloy when higher hardness and strength are needed. Too much silicon adversely affects the hardness, strength, and ductility of the alloy. In order to avoid such adverse effects silicon is restricted to not more than about 2.5% and preferably to not more than about 2.2% or 2.1% in this alloy.
[0014] The alloy contains at least about 0.75% chromium because chromium contributes to the good hardenability, high strength, and temper resistance provided by the alloy. Preferably, the alloy contains at least about 1.0%, and better yet at least about 1.2% chromium. Higher strength can be provided when the alloy contains at least about 1.5% and preferably at least about 1.7% chromium. More than about 2.5% chromium in the alloy adversely affects the impact toughness and ductility provided by the alloy. In the high strength embodiments of this alloy chromium is preferably restricted to not more than about 1.9%. Otherwise, chromium is restricted to not more than about 1.5% in this alloy and better yet to not more than about 1.35%.
[0015] Nickel is beneficial to the good toughness provided by the alloy according to this invention. Therefore, the alloy contains at least about 3.0% nickel and preferably at least about 3.1% nickel. A preferred embodiment of the alloy (e.g., Preferred A) contains at least about 3.7% nickel. When the alloy is balanced to provide higher strength, it preferably contains at least about 4.0% and better yet at least about 4.6% nickel. The benefit provided by larger amounts of nickel adversely affects the cost of the alloy without providing a significant advantage. In order to limit the upside cost of the alloy, the amount of nickel is restricted to not more than about 7%. Thus, for the highest strength embodiment of the alloy (e.g., Preferred C), up to about 5.0% nickel, preferably up to about 4.9% nickel, can be present. In lower strength embodiments (e.g., Preferred A and Preferred B) the alloy contains not more than about 4.5% nickel.
[0016] Molybdenum is a carbide former that is beneficial to the temper resistance provided by this alloy. The presence of molybdenum boosts the tempering temperature of the alloy such that a secondary hardening effect is achieved at about 500° F. Molybdenum also contributes to the strength and fracture toughness provided by the alloy. The benefits provided by molybdenum are realized when the alloy contains at least about 0.4% molybdenum and preferably at least about 0.5% molybdenum. For higher strength, the alloy contains at least about 0.7% molybdenum. Like nickel, molybdenum does not provide an increasing advantage in properties relative to the significant cost increase of adding larger amounts of molybdenum. For that reason, the alloy contains up to about 1.3% molybdenum, better yet not more than about 1.1% molybdenum, preferably not more than about 0.9% molybdenum in the higher strength forms of the alloy (Preferred B and Preferred C). Tungsten may be substituted for some or all of the molybdenum in this alloy. When present, tungsten is substituted for molybdenum on a 2:1 basis.
[0017] This alloy preferably contains at least about 0.5% copper which contributes to the hardenability and impact toughness of the alloy. When higher strength is desired, the alloy contains at least about 0.7% copper. Too much copper can result in precipitation of an undesirable amount of free copper in the alloy matrix and adversely affect the fracture toughness of the alloy. Therefore, not more than about 0.9% and preferably not more than about 0.85% copper is present in this alloy. Copper can be limited to about 0.6% max. when very high strength is not needed.
[0018] Vanadium contributes to the high strength and good hardenability provided by this alloy. Vanadium is also a carbide former and promotes the formation of carbides that help provide grain refinement in the alloy and that benefit the temper resistance and secondary hardening of the alloy. For those reasons, the alloy preferably contains at least about 0.10% and preferably at least about 0.14% vanadium. Too much vanadium adversely affects the strength of the alloy because of the formation of larger amounts of carbides in the alloy which depletes carbon from the alloy matrix material. Accordingly, the alloy may contain up to about 1.0% vanadium, but preferably contains not more than about 0.35% vanadium. In the higher strength embodiments of the alloy (Preferred B and Preferred C), vanadium is restricted to not more than about 0.25% and preferably to not more than about 0.22%. Niobium can be substituted for some or all of the vanadium in this alloy because like vanadium, niobium combines with carbon to form M 4 C 3 carbides that benefit the temper resistance and hardenability of the alloy. When present, niobium is substituted for vanadium on 1.8:1 basis.
[0019] This alloy may also contain a small amount of calcium up to about 0.005% retained from additions during melting of the alloy to help remove sulfur and thereby benefit the fracture toughness provided by the alloy.
[0020] Silicon, copper, vanadium, and when present, niobium are preferably balanced within their above-described weight percent ranges to benefit the novel combination of strength and toughness that characterize this alloy. More specifically, the ratio (% Si+% Cu)/(% V+(5/9)×% Nb) is about 2 to 34. The ratio is preferably about 6-12 for strength levels below about 290 ksi. For strength levels of 290 ksi and above, the alloy is balanced such that the ratio is about 14.5 up to about 34. It is believed that when the amounts of silicon, copper, and vanadium present in the alloy are balanced in accordance with the ratio, the grain boundaries of the alloy are strengthened by preventing brittle phases and tramp elements from forming on the grain boundaries.
[0021] The balance of the alloy is essentially iron and the usual impurities found in commercial grades of similar alloys and steels. In this regard, the alloy preferably contains not more than about 0.01%, better yet, not more than about 0.005% phosphorus and not more than about 0.001%, better yet not more than about 0.0005% sulfur. The alloy preferably contains not more than about 0.01% cobalt. Titanium may be present at a residual level of up to about 0.01% from deoxidation additions during melting and is preferably restricted to not more than about 0.005%. Up to about 0.015% aluminum may also be present in the alloy from deoxidation additions during melting.
[0022] The alloys according to preferred compositions B and C is balanced to provide very high strength and toughness in the hardened and tempered condition. In this regard, the Preferred B composition is balanced to provide a tensile strength of at least about 290 ksi in combination with good toughness as indicated by a K Ic fracture toughness of at least about 70 √in. In addition, the Preferred C composition is balanced to provide a tensile strength of at least about 310 ksi in combination with a K Ic fracture toughness of at least about 50 √in for applications that require higher strength and good toughness.
[0023] No special melting techniques are needed to make the alloy according to this invention. The alloy is preferably vacuum induction melted (VIM) and, when desired as for critical applications, refined using vacuum arc remelting (VAR). The alloy can also be arc melted in air (ARC) if desired. After ARC melting, the alloy may be refined by electroslag remelting (ESR) or VAR.
[0024] The alloy of this invention is preferably hot worked from a temperature of up to about 2100° F., preferably at about 1800° F., to form various intermediate product forms such as billets and bars. The alloy is preferably heat treated by austenitizing at about 1585° F. to about 1735° F. for about 1-2 hours. The alloy is then air cooled or oil quenched from the austenitizing temperature. When desired, the alloy can be vacuum heat treated and gas quenched. The alloy is preferably deep chilled to either −100° F. or −320° F. for about 1-8 hours and then warmed in air. The alloy is preferably tempered at about 500° F. for about 2-3 hours and then air cooled. The alloy may be tempered at up to 600° F. when an optimum combination of strength and toughness is not required.
[0025] The alloy of the present invention is useful in a wide range of applications. The very high strength and good fracture toughness of the alloy makes it useful for machine tool components and also in structural components for aircraft, including landing gear. The alloy of this invention is also useful for automotive components including, but not limited to, structural members, drive shafts, springs, and crankshafts. It is believed that the alloy also has utility in armor plate, sheet, and bars.
WORKING EXAMPLES
[0026] Two 400 lb. heats having the weight percent compositions shown in Table 1 below were prepared for evaluation as follows. Both heats were vacuum induction melted and then cast as
[0000] TABLE 1 Element Heat 1 Heat 2 C 0.35 0.41 Mn 1.17 1.18 Si 2.00 2.02 P 0.008 0.007 S <0.0005 0.0006 Cr 1.74 1.74 Ni 3.24 4.75 Mo 0.77 0.76 Cu 0.79 0.79 Co <0.01 Ti 0.006 0.006 Al 0.007 0.008 N 0.0032 0.0036 O 0.0010 <0.0010 V 0.19 0.19 Fe Bal. Bal.
7.5 inch square ingots. The ingots were heated at 2300° F. for a time sufficient to homogenize the alloys. The ingots were then hot worked from a temperature of 1800° F. to 3½ inch×5 inch bars. The bars were then reheated to 1800° F. and a portion of each bar was further hot worked to a cross section of 1½ inches×4⅝ inches. The hot working was carried out in steps with reheating of the intermediate forms as needed. After forging, the bars were allowed to cool to room temperature in air. The cooled bars were each then cut into two pieces at the junction between the two section sizes. The bar pieces were annealed at 1250° F. for 8 hours and then cooled in air.
[0027] Standard tensile, Charpy V-notch, and fracture toughness, and hardness test specimens were prepared from the bar pieces with both longitudinal and transverse orientations. The test specimens were heat treated as follows for testing. The specimens of Heat 1 were austenitized in a vacuum furnace at 1685° F. for 1.5 hours and then gas quenched. The as-quenched specimens were deep chilled at −100° F. for 8 hours and then warmed to room temperature in air. Finally, the specimens were tempered at 500° F. for 2 hours and then cooled in air from the tempering temperature. The specimens of Heat 2 were austenitized in a vacuum furnace at 1735° F. for 2 hours and then gas quenched. The as-quenched specimens were deep chilled at −100° F. for 8 hours and then warmed to room temperature in air. Finally, the specimens were tempered at 500° F. for 2 hours and then cooled in air from the tempering temperature.
[0028] The results of room temperature tensile, Charpy V-notch, and K Ic fracture toughness testing are shown in Tables 2A and 2B below including the 0.2% offset yield strength (Y.S) and ultimate tensile strength (U.T.S.) in ksi, the percent elongation (% El.) and percent reduction in area (% R.A.), the Charpy V-notch impact strength (CVN) in ft-lbs, the rising step load K Ic fracture toughness in ksi√in, and Rockwell C-scale hardness (HRC). The rising step load fracture toughness test was conducted in accordance with ASTM Standard Test Procedures E399, E812, and E1290. Table 2A shows the results for Heat 1 and Table 2B shows the results for Heat 2.
[0000]
TABLE 2A
Orien-
%
tation
Sample
Y.S.
U.T.S.
% El.
R.A.
CVN
K Ic
HRC
Longi-
1
235.8
297.2
11.0
44.9
23.1
73.6
tudinal
2
235.7
296.8
12.7
50.7
22.0
74.8
Average
235.7
297.0
11.9
47.8
22.6
74.2
55.1
Transverse
1
*
*
*
*
22.3
75.0
2
233.8
296.5
11.1
40.8
21.6
73.3
Average
233.8
296.5
11.1
40.8
22.0
74.2
55.2
* = Not Included in Averages - Cause of low properties not known.
[0000]
TABLE 2B
Orien-
%
tation
Sample
Y.S.
U.T.S.
% El.
R.A.
CVN
K Ic
HRC
Longi-
1A
244.2
312.7
10.9
44.1
19.2
56.8
tudinal
2A
244.5
312.6
11.9
48.8
16.8
55.7
56.3
Longi-
1B
246.9
313.1
10.7
44.1
16.8
57.5
tudinal
2B
245.0
312.1
11.6
50.4
17.9
59.3
56.2
Average
245.1
312.6
11.3
46.9
17.7
57.3
56.3
Transverse
1A
243.9
311.7
10.8
42.2
14.1
55.2
2A
**
**
**
**
14.3
57.6
56.0
Transverse
1B
246.7
312.2
10.6
41.9
15.4
56.4
2B
246.5
312.2
10.9
43.4
15.0
56.9
56.2
Average
245.7
312.1
10.8
42.5
14.7
56.5
56.1
** = Tensile specimen was cracked
[0029] The terms and expressions which are employed herein are used as terms of description and not of limitation. There is no intention in the use of such terms and expressions of excluding any equivalents of the features shown and described or portions thereof. It is recognized that various modifications are possible within the invention described and claimed herein. | A high strength, high toughness steel alloy is disclosed. The alloy has the following weight percent composition.
Element C 0.30-0.47 Mn 0.8-1.3 Si 1.5-2.5 Cr 1.5-2.5 Ni 3.0-5.0 Mo + ½ W 0.7-0.9 Cu 0.70-0.90 Co 0.01 max. V + ( 5/9) × Nb 0.10-0.25 Ti 0.005 max. Al 0.015 max. Fe Balance
Included in the balance are the usual impurities found in commercial grades of steel alloys produced for similar use and properties including not more than about 0.01% phosphorus and not more than about 0.001% sulfur. Also disclosed is a hardened and tempered article that has very high strength and fracture toughness. The article is formed from the alloy having the broad weight percent composition set forth above. The alloy article according to this aspect of the invention is further characterized by being tempered at a temperature of about 500° F. to 600° F. | 2 |
REFERENCE TO PENDING APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application, Ser. No. 61/081,153 filed Jul. 16, 2008.
REFERENCE TO MICROFICHE APPENDIX
[0002] This application is not referenced in any microfiche appendix.
BACKGROUND OF THE INVENTION
[0003] This invention relates to a shower door apparatus, and more specifically to a shower door extension apparatus the expands the usable space during the taking of a bath or shower.
[0004] The traditional shower door that is attached a bathtub is aligned in-line with the edge of the top rim of the bath tub. This can make a user feel claustrophobic. Many people may find it difficult to wash or shave in such confined areas.
[0005] The prior art discloses a curved shower rod that allows for additional space near the top of the shower curtain. However, the effectiveness of these prior art rods is limited because such rods do not address the narrowness of the tub near the tub's rim. Thus there is a need for a more efficient and effective shower door extension apparatus.
SUMMARY OF THE INVENTION
[0006] The inventive shower door extension apparatus described herein satisfies the needs set out above. This device has an efficient design and it is effective when used.
[0007] An aspect of the present invention includes a shower door apparatus that is secured to the top rim of a bath tub. The shower door apparatus includes a base plate and shower door frame assembly. The base plate is secured to the top rim of the bathtub and extends outward and beyond the bath tub. The shower door frame assembly is secured to the base plate near the distal edge, herein referred to as the extension edge. The inclusion of the base plate and the shower door frame assembly, the usable space within a bathtub can be increased.
[0008] The extension edge can either be substantially parallel to its opposite edge, herein referred to as the bathtub edge, or can be curved. One such curvature is a concave curve relative toward the bath tub.
[0009] One aspect of the shower door frame assembly includes having a shower door frame and at least one shower door. The shower door frame can be of standard shower door frame having tracks therein to slidably engage the one or more shower doors.
[0010] One aspect of the base plate includes having a water run-off portion. This portion is located along the top surface of the base plate and is sloped downward toward said bathtub edge. The slope allows for water to run off into the bath tub.
[0011] Another aspect of the base plate includes having at least one base plate support secured to the bottom surface and said bath tub. This aspect can give additional support to the base plate.
[0012] Upon reading the included description, various alternative embodiments will become obvious to those skilled in the art. These embodiments are to be considered within the scope and spirit of the subject invention, which is only limited by the claims which follow and their equivalents.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a perspective view of an embodiment of the present invention.
[0014] FIG. 2 is a back view of an embodiment of the present invention as shown in FIG. 1 .
[0015] FIG. 3 is a right side view of an embodiment of the present invention as shown in FIG. 1 .
[0016] FIG. 4 is a left side view of an embodiment of the present invention as shown in FIG. 1 .
[0017] FIG. 5 is a top view of an embodiment of the present invention as shown in FIG. 1 .
[0018] FIG. 6 is a cut-away side view of an embodiment of the base plate along line BB as shown in FIG. 1 .
[0019] FIG. 7 is a cut-away side view of an embodiment of the present invention along line AA as shown in FIG. 1 .
[0020] FIG. 8 is a cut-away side view of an embodiment of the present invention along line AA as shown in FIG. 1 showing an embodiment of a base plate support.
[0021] FIG. 9 is a perspective view of an additional embodiment of the present invention.
[0022] FIG. 10 is a top view of an embodiment of the present invention as shown in FIG. 9 .
[0023] FIG. 11 is a side view of an embodiment of the base plate as shown in FIG. 9 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0024] The following detailed description shows the best currently contemplated modes of carrying out the invention. The description is not to be taken in a limiting sense, but is made for the purpose of illustrating the general principles of the invention and the best mode for practicing the invention, since the scope of the invention is best defined by the appended claims. The invention is capable of other embodiments and of being practiced or carried out in a variety of ways. It is to be understood that the phraseology and terminology employed herein are for the purpose of description and not of limitation.
[0025] As shown by the figures, embodiments of the inventive shower door apparatus is described herein. As illustrated in FIGS. 1-8 , a first embodiment of the inventive shower door apparatus 20 is shown secured to the top rim 24 of a bathtub 22 . Embodiment 20 comprises a base plate 30 having a top surface 40 , a bottom surface 38 , a bathtub edge 34 and an extension edge 36 . The portion of bottom surface 38 that is proximate to the bathtub edge 34 is secured to top rim 34 of the bathtub 22 by any form of adhesives, glues or any other known securing compound.
[0026] Base plate 30 extends outward, and beyond, bathtub 22 , such that extension edge 36 is distal to bathtub 22 . As illustrated by embodiment 20, extension edge 36 is shown to be curved, with such curve being concave relative to the bathtub 22 . The amount of curvature can be adjusted based on the actual size of the bathtub and surrounding environment. The curvature shown in embodiment 20 is shown as a 6×60 curvature. By this it is meant that when the base plate 30 has a 60 inch length the maximum width between the extension edge 36 and the bathtub edge 34 is 6 inches. However, those skilled in the art will recognize the actual dimensions and type of curvature of this embodiment is illustrative and is not meant to be limiting.
[0027] As shown in FIG. 6 , an embodiment of the top surface 40 of base plate 30 is shown having a water run-off portion 44 . This water run-off portion 44 is sloped downward toward the bathtub edge 34 to aid in the movement of water. Further, base plate 30 is shown having a shower door frame assembly mounting surface 42 located proximate the extension edge 36 . The mounting surface allows for a relatively flat surface, i.e. being relatively parallel with the bottom surface 38 of the base plate 30 for the shower door frame assembly 20 to be mounted thereto while allowing for water run-off via the water run-off portion 44 .
[0028] Also shown in the Figures is an embodiment of the shower door frame assembly 50 . This assembly 50 is secured to the top surface 40 of base plate 30 proximate to extension edge 36 . By being secured to the distal end of base plate 30 , the usable space from the top rim 24 of the bathtub 22 to the top of the shower door frame assembly 20 is increased.
[0029] As illustrated, shower door frame assembly 50 comprises a shower door frame 52 and two shower doors 54 . Those skilled in the art will recognize that the number of shower doors in this embodiment is illustrative and is not meant to be limiting.
[0030] Shower door frame 52 is shown comprising a top bar 56 , a bottom bar 58 and first side support 60 and a second side support 62 . Tracks are included therein sufficient dimensioned to allow the shower doors 54 to slidably engage the tracks.
[0031] Further, in this embodiment 20, a bottom bar 58 is secured to the top surface 40 is illustrated. The manner in which bottom bar 58 and top surface 40 are secured can be by adhesives, snap-rivets, or any other manner of securing these items together.
[0032] As illustrated in FIG. 8 , an optional base plate support 70 is shown. This base plate support 70 is secured to the bottom surface 38 of base plate 30 and in contact with the outer surface of bathtub 22 .
[0033] As illustrated by FIGS. 9-11 , a second embodiment 120 discloses the inventive shower door apparatus as set out above but having an extension edge 136 that is substantially parallel to bathtub edge 134 .
[0034] While embodiments of the present invention have been illustrated and described, such disclosures should not be regarded as any limitation of the scope of our invention. The true scope of our invention is defined in the appended claims. Therefore, it is intended that the appended claims shall be construed to include both the preferred embodiment and all such variations and modifications as fall within the spirit and scope of the invention. | A shower door apparatus is disclosed being secured to the top rim of a bath tub. The shower door apparatus has a base plate extending outward from, and beyond, the top rim of the bath tub. A shower door frame assembly having at least one shower door is secured to the base plate near the edge distal to the bath tub. | 0 |
TECHNICAL FIELD OF THE INVENTION
The present invention is directed, in general, to a method of manufacturing a copolymer and, more specifically, to a method of manufacturing a poly vinylbenzene in the presence of a cross-linking agent and a chain transfer agent.
BACKGROUND OF THE INVENTION
The polymerization of styrene is a very important industrial process that supplies materials used to create a wide variety of polystyrene-containing articles. This expansive use of polystyrene results from the ability to control the polymerization process. Thus, variations in the polymerization process conditions are of utmost importance since they in turn allow control over the physical properties of the resulting polymer. The resulting physical properties determine the suitability of a polystyrene for a particular use. For a given product, several physical characteristics must be balanced to achieve a suitable polystyrene material. Among the properties that must be controlled and balanced are weight averaged molecular weight (M w ) of the polymer, molecular weight distribution (MWD), melt flow index (MFI), and the storage modulus (G′).
U.S. Pat. No. 5,540,813 by Sosa, et. al. (Sosa '813), which is incorporated herein by reference, discloses a process for preparing monovinyl aromatic polymers, such as polystyrene, which utilizes a combination of sequentially ordered multiple reactors, heat exchangers and devolatilizers to strictly control polymer properties such as the molecular weight distribution and melt flow index.
While the Sosa '813 patent discloses methods for controlling the molecular weight distribution and melt flow index, it does not address the relationship between the molecular weight and the storage modulus. This relationship is of particular importance in polymer foam applications. Such foam applications require high molecular weight polymers having a high storage modulus. It is thought that the storage modulus is related to the degree of branching along the polymer chain. As the degree of branching increases, the likelihood that a branch connects two different polymer chains increases. This inter-chain interaction is known as cross-linking. A polymer product having a higher degree of branching or cross-linking tends to have a higher storage modulus and, therefore, better foam stability characteristics.
Methods for preparing branched polymers are well-known in the art. For example, the preparation of branched polystyrene by free radical polymerization has been reported in U.S. Pat. Nos. 5,473,031 and 5,663,253 issued to Tinetti, et. al., and Pike, et. al., respectively. Both methods increase the branching in the devolatilization step and produce a polymer with an undesirably low molecular weight.
Rather than employing free radical polymerization, U.S. Pat. No. 4,918,159 issued to Idemitsu teaches the use of multi-functional mercaptans to form branched polymers. While materials having an acceptable molecular weight can be prepared by this method, these products are unacceptable for foam applications due to their undesirable flow properties.
The properties of randomly branched polystyrene prepared in the presence of divinylbenzene have been reported by Rubens (L. C. Rubens, J. of Cellular Physics, pp 311-320, 1965). However, polymers having a useful combination of molecular weight and cross-linking are not attainable. At low concentrations of divinylbenzene, low molecular weight polymers having little branching result. However, higher concentrations of the cross-linking agent result in excessive cross-linking and concomitant gel formation. While increasing cross-linking generally correlates with the polymer storage modulus, formation of a gel is highly undesirable in industrial polystyrene processes. Similar results and problems were reported by Ferri and Lomellini (J. Rheol. 43(6), 1999).
Thus what is needed in the art is a process for monovinyl aromatic polymers that produces a branched or very slightly cross-linked product that has a high molecular weight, a high storage modulus at foaming and is suitable for foam applications.
SUMMARY OF THE INVENTION
To address the deficiencies of the prior art, the present invention provides a method of producing a copolymer. In an advantageous embodiment, the method comprises placing a vinylbenzene, such as styrene, in a reactor, placing a cross-linking agent, such as divinylbenzene in the reactor, placing a chain transfer agent, such as mercaptan, in the reactor and forming a poly vinylbenzene in the presence of the cross-linking agent and the chain transfer agent. In this embodiment, the concentration of the cross-linking agent ranges from about 150 ppm to about 400 ppm and a concentration of the chain transfer agent ranges from about 100 to about 400 ppm.
The foregoing has outlined, rather broadly, preferred and alternative features of the present invention so that those skilled in the art may better understand the detailed description of the invention that follows. Additional features of the invention will be described hereinafter that form the subject of the claims of the invention. Those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiment as a basis for designing or modifying other structures for carrying out the same purposes of the present invention. Those skilled in the art should also realize that such equivalent constructions do not depart from the spirit and scope of the invention in its broadest form.
BRIEF DESCRIPTION OF THE DRAWINGS
For a more complete understanding of the invention, reference is now made to the following descriptions taken in conjunction with the accompanying drawing, in which:
FIG. 1 illustrates a schematic representation of the polymerization system that can be used in conjunction with the present invention;
FIG. 2 illustrates graphical data indicating the storage modulus as a function of temperature for a control group and an experimental group of polymer products; and
FIG. 3 illustrates graphical data indicating the storage modulus as a function of temperature for several of polymer products.
DETAILED DESCRIPTION
In the present invention, polymerization processes for the preparation of copolymers, such as polyvinylbenzene copolymers, are disclosed. The present invention is particularly useful with polymerization systems such as those disclosed in the aforementioned Sosa '813 patent.
Referring initially to FIG. 1, there is illustrated a schematic representation of the polymerization system 100 of the present invention having a stirred tank reactor 110 . Reactor 110 may comprise a series of reactors for manufacturing polystyrene. Flowlines 120 , 121 , and 122 link the reactor 110 with storage reactant containers 140 , 150 , and 160 .
In an embodiment of the present invention, flowline 120 transports a vinylbenzene from storage container 140 to the reactor 110 . Also, in this embodiment flowlines 121 and 122 transport a cross-linking agent and a chain transfer agent from storage containers 140 and 150 , respectively, to the reaction vessel 110 where the vinylbenzene, cross-linking agent and chain transfer agent are combined.
In one embodiment the vinylbenzene may be styrene and a preferred cross-linking agent may be a divinylbenzene. one who is killed in the art understands that substituted vinylbenzene and substituted divinylbenzene molecules or other tri- or tetra-functional monomers may also be employed. The concentration of the cross-linking agent in the mixture may vary. However, in a preferred embodiment, the cross-linking agent's concentration may range from about 200 ppm to about 400 ppm. If the concentration of the cross-linking agent is too low the molecular weight, M w of the resulting polymer may be too low, and if the concentration of the cross-linking agent is too high an undesirable gel may form.
The chain transfer agent is preferably a member of the mercaptan family. Particularly useful mercaptans include n-octyl mercaptan, t-octyl mercaptan, n-dodecyl mercaptan, t-dodecyl mercaptan, tridecyl mercaptan, tetradecyl mercaptan, and hexadecyl mercaptan. In advantageous embodiments, the concentration of the mercaptan may range from about 100 ppm to about 400 ppm. Again, if the concentration of chain transfer agent is too low the storage modulus, G′ is not improved. However, if the concentration is too high the molecular weight Mw of the resulting polymer is too low to used to manufacture certain products.
In an exemplary embodiment, the reactor 110 containing the vinylbenzene, cross-linking agent and the chain transfer agent is heated sufficiently to cause a polymerization reaction. The polymerization may alternatively be chemically initiated. in either case, the reactor 110 may also include a diluent. One particular diluent is ethyl benzene. Such processing parameters and initiators are well known to those skilled in the art. However, in a particular embodiment the reactor 110 may be heated to a temperature ranging from about 100° C. to about 180° C. and for a period ranging from about 4 hours to about 6 hours. The particular conditions of the heating process may be determined by monitoring the percent conversion in reactor 110 . Those who are skilled in the art appreciate that the percent conversion indicates the amount of polymer products that have been produced. In a preferred embodiment, the percent conversion in reactor 110 is approximately 70%. After passing through the reactor 110 , the resulting polymer mixture enters the heat exchanger 170 through flowline 123 . Heat exchanger 170 is preferably an upflow heat exchanger and may be operated at a temperature sufficient to induce polymerization, about 160° C. The polymer then flows from heat exchanger 170 through flowline 124 to the downflow heat exchanger 180 . Downflow heat exchanger 180 may be maintained at a temperature of about 245° C. and may be situated in a flash devolatilization tank 181 having a vapor removal line 182 and maintained at a pressure in the range of about 20 torr to about 200 torr.
After having been at least partially devolatilized in the devolatilization tank 181 , the polymer mixture passes through flow line 125 to a second devolatilizer 190 having a hoop falling strand configuration and is operated at a pressure of about less than 1 Torr to about 20 Torr. Volatile components are removed through vapor line 195 . Then, flowline 126 transports the polymer mixture from devolatilizer 190 to a finishing operation such as pelletizer 200 . More details of the operation of the reactor system illustrated in FIG. 1 may be found in Sosa '813.
EXAMPLES
Table I illustrates specific examples taken from pilot plant operations utilizing the process of the present invention. For example, a control experiment was performed wherein neither a cross liking agent nor a chain transfer agent where present during the polymerization. After devolatilization, the weight averaged molecular weight of the product polystyrene is 388,000 and the storage modulus G′ is 79,000 Pa at 145° C.
The effect of the cross-linking agent on the polymer product of this process was investigated in Experiment 1. In this example styrene was polymerized in the presence of divinylbenzene at a concentration of 200 ppm and no chain transfer agent was present in the mixture. The weight averaged molecular weight increased to 660,000. However, the storage modulus decreased to 70,000 Pa at 145° C.
It had been believed that the presence of a chain transfer agent in a polymerization would effect the amount of cross-linking and therefore, lower the storage modulus of the resulting polymer. However, when styrene was polymerized in the presence of 250 ppm of divinylbenzene and 200 ppm of n-dodecyl mercaptan, the weight averaged molecular weight remained high at 652,000 and the storage modulus unexpectedly increased to 85,000 Pa at 145° C.
Several other conditions were employed in Experiments 3, 4, and 5 in an effort to optimize the molecular weight and storage modulus of the polymer product. Styrene was polymerized in the presence of 250 ppm of divinylbenzene and 400 ppm of n-dodecyl mercaptan where the weight averaged molecular weight decreased to 587,000. Under these conditions the storage modulus decreased slightly to 78,000 Pa at 145° C. Changing the concentration of divinylbenzene and n-dodecyl mercaptan to 350 ppm and 200 ppm, respectively, produced a polystyrene with a weight averaged molecular weight of 735,000 and a storage modulus of 75,000 Pa at 145° C. When the concentrations of divinylbenzene and n-dodecyl mercaptan were 350 ppm and 400 ppm, respectively, the resulting polystyrene had a weight averaged molecular weight of 733,000 and a storage modulus of 80,500 Pa at 145° C. The effect of higher concentrations of chain transfer agent was also explored in Experiments 6 and 7. Under these conditions both the molecular weight of the polymer and the storage modulus were reduced.
The effects of higher concentrations of chain transfer agent were also explored. As Table I indicates, concentrations of n-dodecyl mercaptan of 500 ppm resulted in polymer products having unacceptably low molecular weights and storage moduli.
TABLE I
Control
1
2
3
4
5
6
7
divinyl-benzene
0
200
250
250
350
350
150
0
(ppm)
n-dodecyl
0
0
200
400
200
400
500
500
mercaptan (ppm)
M W (in thousands)
388
660
652
587
735
733
324
249
G′ (KPa) at 145° C.
79.0
70.0
85.0
78.0
75.0
80.5
50
48
FIGS. 2 and 3 show the storage modulus as a function of temperature for several of the polymer products prepared as indicated by Table I. Thus, as Table I and FIGS. 2 and 3 indicate, the various parameters can be varied to achieve desired levels of polymer properties. Certain properties, for instance the molecular weight or storage modulus, can be optimized for a particular use by adjusting either the cross-linking agent or chain transfer agent or both. In this process the presence of a cross-linking agent and a chain transfer agent increases the molecular weight to desired levels without gel formation problems and unexpectedly maintains or increases the storage modulus.
Although the present invention has been described in detail, those skilled in the art should understand that they can make various changes, substitutions and alterations herein without departing from the spirit and scope of the invention in its broadest form. | The present invention provides a method of producing a copolymer. The method comprises placing a vinylbenzene, such as styrene, in a reactor, placing a cross-linking agent, such as divinylbenzene in the reactor, placing a chain transfer agent, such as mercaptan, in the reactor and forming a poly vinylbenzene in the presence of the cross-linking agent and the chain transfer agent. In this embodiment, the concentration of the cross-linking agent ranges from about 150 ppm to about 400 ppm and a concentration of the chain transfer agent ranges from about 100 to about 400 ppm. | 2 |
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims the priority to Chinese Patent Application No. CN201410064305.9, filed Feb. 25, 2014, in the State Intellectual Property Office of P.R. China, which is hereby incorporated herein in its entirety by reference.
FIELD
[0002] The present invention belongs to the ramie technical field and relates to, in particular, a method for degumming the ramie phloem fibers.
BACKGROUND
[0003] Global fossil resources are going to be exhausted, and the environmental pollution is increasingly severe. Solving the problems of the resources and environment is the important task for the economic sustainable development in 21 st century. However, the chemical fibers with petroleum as the starting material comprise about 67% in the total amount of the textile industry in China, the yield of which is over 50% in the world. It will be faced a severe problem in ensuring the petroleum supply in a long term and steadily. It has been an international trend to change the present situation that the petroleum resources are deeply relied on by the chemical fiber industry in China or even the world, and develop the utilization of the natural fibers. 2009 has been designated as the “International Year of Natural Fibers”. The usage of natural fibers has increased by 8% and 15% every year in the world and China, respectively. The yield of cotton, the main natural fibers in China, is about 6 million tons per year with a gap of about 6 to 8 million tons that is not likely to be compensated by planting cotton in the cereals cropland instead. The productivity has reached the plateau for other natural fibers in China, such as silk and wool, both of which have a yield of 100,000 tons per year. The bast fiber crops are cultivated in extensive conditions and suitable to be planted in various places, and have a great potential to be developed in the industrial scale. The most advantageous bast fiber crop is ramie. From of old, ramie is the typical crop mainly used in textile in China and known as “China grass” overseas. China has 90% of the ramie yield in the world and extremely high international competitive capacity that 80% of the ramie products are outputted to comprise over 60% of the global textile trade volume. There are 459 relatively large ramie textile and/or ramie textile manufacturing enterprises in China, offering nearly 1 million jobs.
[0004] The ramie industry is the traditional national industry in China and belongs to the labour intensive industries. In China, the employees in the ramie industry chain are up to several millions. The ramie dress has the advantages such as being stiff and neat, elegant, light, cool, breathable and anti-bacterial, and belongs to top grade consumer goods. The utilization of ramie fiber resources is turning from the traditional textile field to the biomass energy sources and biomaterials. Both the ramie materials and the ramie products have a broad market prospect.
[0005] The degumming of the ramie is an important step in the ramie processing. At present in China, most of the ramie processing enterprises adopt the chemical degumming, involving acid immersing, alkali boiling, and hammering-and-washing steps, which not only renders the degumming process long, the process steps complicated, the energy and water consumption high, and the pollution severe, but also causes damage to the ramie fibers and lowers the fiber quality. The biological degumming is focused in the clean production technology studies of the phloem fibers of the bast fiber crops at home and abroad, and is by the mechanism that the microorganisms and their secreted extracellular enzyme(s) are utilized to allow a series of reactions occur in relatively mild conditions so as to degrade the ramie phloem gum and release the fibers. The biological degumming is believed to be most possibly used in production practice in place of chemical degumming due to the avoidance of strong acids and alkalis, saving energy and water and little environmental pollution. The biological degumming of the ramie has been studied for over 80 years in China. Mainly, the superior degumming bacteria are screened from the nature and incubated into high-efficient degumming strains by physical or chemical mutagenesis, and then, the scaled-up bacterium-and-enzyme mixed liquor or the critical degumming enzyme(s) isolated therefrom is used for degumming. In the past decades, a number of degumming bacteria have been obtained from the microorganism resources, wherein the Erwinia carotovora strain T85-260 screened by the Institute of Bast Fiber Crops, Chinese Academy of Agricutral Sciences, the Bacillus alcalophilus strain screened by Wuhan University, the Bacillus alcalophilus strain screened by Shandong University, and the wild Bacillus cereus strain screened by Qingdao Continent Biotech Co., Ltd have ever been proceeded to the production test stage, and the others are still in the laboratory stage.
[0006] In the last 90s, the commercial production test has been performed for the biological degumming technologies. The patent “A technology for degumming the ramie jointly by bacteria and chemistry” (CN85103481) has been extended in 5 enterprises, and the patent “A process and equipment for biologically degumming the ramie” (CN95112564.8) has been tested for production in 6 enterprises including the Number 2 and 3 Ramie Textile Factories of Ruanjiang City, Hunan Province. The attempts failed mainly because the seed production technology is difficult to be mastered and the degumming capacity is not sufficient. The patent CN01106884.2 has been tested in Number 2 Ramie Textile Factory of Ruanjiang City, and the patent CN97109044.0 has been tested for production in Jiangxi Enda Hometextile Co., Ltd. These tests were in the joint manner of biological-and-chemical degumming. The large-scale production test of purely biological degumming was started in 2007 in the Star Textile Factory of Ruanjiang, Hunan. However, it has now been forced to change to joint biological-and-chemical degumming, which is mainly because the degummed ramie by purely biological degumming is not ideal and the products produced using the same are not welcome in the market.
SUMMARY OF THE INVENTION
[0007] The technical problem to be solved by the present invention is to provide a chain, continuous and no-waste technology for degumming and fiber-separating the ramie, which solves the problems resulted from the discharge of the residual liquid after the traditional batch single-tank treatment, such as high consumption of chemicals and the production of highly concentrated wastewater, to reach the bast fiber processing with zero discharge and solve the problems, such as high consumption of water and severe pollution, in the existing ramie degumming process.
[0008] The present invention solves the technical problem by the following solution:
[0009] A chain, continuous and no-waste method for degumming and fiber-separating the ramie according to the present invention, including:
[0010] (1) waste alkali bath step, in which the raw fibers are immersed in the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching at ambient temperature for 8 h;
[0011] (2) anaerobic circle step, in which the raw fibers treated in the waste alkali bath are immersed in the anaerobic water pool in a bath ratio of 1:15 to 25, and washed at ambient temperature for 8 h;
[0012] (3) aerobic circle step, in which the raw fibers washed in the anaerobic water pool are immersed in the aerobic water pool in a bath ratio of 1:15 to 25, and washed at ambient temperature for 8 h;
[0013] (4) alkali-hydrogen peroxide one bath scouring-bleaching step, in which the raw fibers treated in the aerobic circle step are immersed in a solution comprising 1 to 10 g/L NaOH and 0 to 2 g/L H 2 O 2 in a bath ratio of 1:15 to 25, and reacted at the temperature of 70 to 100° C. for 2 h;
[0014] (5) fiber-separating and washing step, in which the raw fibers washed in the alkali-hydrogen peroxide one bath scouring-bleaching step are treated by the fiber-separating and washing device with a washing time of 4 h, which step can be performed either by rolling and rubbing manually or in a mechanical way;
[0015] (6) bio-enzyme washing step, in which the raw fibers treated in the fiber-separating and washing step are immersed in a solution having a cellulose concentration of 5 to 30 U in a bath ratio of 1:15 to 25 and reacted at the temperature of 55° C. for 2 h to reach the no-waste degumming and fiber-separating of the raw ramie fibers, depending on the quality requirements.
[0016] According to the present invention, a disc is used as the device units in a chain connection in the process of the no-waste degumming and fiber-separating of the raw ramie fibers, rendering a continuous operation; the ramie degumming process and the degumming wastewater treatment are performed integratively, and the effluent from the alkali-hydrogen peroxide one bath scouring-bleaching is introduced into the waste alkali bath and used for the immersion of the raw fibers; the water used in the anaerobic washing step is circulated with the anaerobic pool for sewage treatment; the water used in the aerobic washing step is circulated with the aerobic pool for sewage treatment; the effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing are recycled after treatment in the sewage treatment system, and no sewage is discharged.
[0017] The effluent from the alkali-hydrogen peroxide one bath scouring-bleaching is highly polluted wastewater, and a majority of the COD therein can be precipitated by flocculation after being used in the waste alkali bath, to form the sludge to be treated separately, and the supernatant is then discharged into the sewage treatment system so as to reduce the load of the subsequent sewage treatment system.
[0018] The degumming process is a continuous disk operation, and the chemicals in the alkali-hydrogen peroxide one bath scouring-bleaching step can be repeatedly used for many times to reduce the discharge of the degumming chemicals every time.
[0019] The soluble gum can be partially squeezed out from the ramie in the mechanical squeezing and water flow washing process to fiber-separate the raw fibers partially.
[0020] The cellulase is a normal cellulase, an acidic cellulase, a neutral cellulase or an alkaline cellulase, and not limited by the pH value.
[0021] The fiber-separating and washing device can be the ramie fiber back washing device Model ZMXFC-1 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd.
[0022] The present invention has the following advantages as compared to the prior art:
[0023] 1) The existing chemical degumming process is a batch operation, and the solution containing sodium hydroxide and degumming aids is discharged directly every time after the completion of degumming, which leads to the failure of recycling the degumming chemicals and the discharge of a large amount of highly concentrated wastewater. The degumming process of the present invention is a continuous disc operation, and the chemicals in the alkali-hydrogen peroxide one bath scouring-bleaching step are repeatedly used for many times, which reduces the discharge of the degumming chemicals every time, and perform the step with most severe pollution separately to reduce the load of the subsequent sewage treatment systems.
[0024] The separate performation of the step with most severe pollution in the degumming process reduces the difficulty of treating the wastewater coupled with the same. The effluent from the alkali-hydrogen peroxide one bath scouring-bleaching is highly polluted wastewater, and a majority of the COD therein are precipitated by flocculation after being used in the waste alkali bath, to form the sludge to be treated separately, and the supernatant is then discharged into the sewage treatment system so as to reduce the COD concentration in the influent of the degumming wastewater treatment system and reduce the treatment difficulty and the treatment cost.
[0025] 2) The existing biological degumming process suffers from the product homogeneity problem because the seed activation, amplifying culture, and degumming needs to be performed again in every degumming, which cannot ensure the complete consistency between the seed concentrations used in every time and thus results the significantly different batches of degummed ramie by biological degumming. In the present invention, the water used in the anaerobic washing step is circulated with the anaerobic pool for sewage treatment, and the water used in the aerobic washing step is circulated with the aerobic pool for sewage treatment. Since the degumming wastewater treatment is continuously performed, the anaerobic and aerobic washing steps not only wash away partially the alkali liquid on the raw ramie fiber left after the waste alkali bath step, but also have the effect of the biological treatment, without suffering from the homogeneity problem of the microorganism treatment.
[0026] 3) The severe pollution problem with the ramie degumming is solved. For the production of every one ton of the degummed ramie, the present method discharges barely the degumming wastewater and reaches the raw ramie fiber degumming process with zero discharge as compared to the discharge of 500 tons of wastewater for the production of one ton of the degummed ramie in the traditional degumming processes.
[0027] 4) The present invention uses a disc as the degumming device unit and connects each of the degumming steps by a chain to degum continuously. The degumming is performed in a coupled physical, chemical, and biological way and the degumming operation is performed gradually. The degumming efficiency is improved and the degumming cost is reduced.
[0028] In a word, the ramie degumming process and the degumming wastewater treatment are performed integratively according to the present invention. The degumming wastewater is entirely recycled after treatment, without sewage discharge.
DESCRIPTION OF THE DRAWINGS
[0029] FIG. 1 is a schematic view of the process flow of the chain, continuous and no-waste technology for degumming and fiber-separating the ramie according to the present invention.
[0030] FIG. 2 is a schematic view of the structure of the production line.
[0031] FIG. 3 is a schematic view of the sequencing batch decorticator in FIG. 2 .
[0032] FIG. 4 is a schematic view of the automatic stem separation machine in FIG. 2 .
[0033] FIG. 5 is the roller type transport platform in FIG. 2 .
[0034] FIG. 6 is a schematic view of the stamping machine in FIG. 2 .
[0035] FIG. 7 is a schematic view of the structure of the washing and degumming section in FIG. 2 .
[0036] FIG. 8 is a schematic view of the structure of the ramie fiber cleaning unit in FIG. 2 .
[0037] In the figures: 1 . ramie sorting platform; 2 . sequencing batch decorticator; 3 . automatic ramie stem separation machine; 4 . first mechanical hand; 5 . roller type transport platform; 6 . stamping machine; 7 . second mechanical hand; 8 . degumming and washing device; 9 . third mechanical hand; 10 . ramie fiber back washing device; 11 . bast fiber collecting frame of the sequencing batch decorticator; 12 . stem inlet of the sequencing batch decorticator; 13 . stem inlet of the automatic ramie stem separation machine; 14 . bast fiber collecting and transporting configuration of the automatic ramie stem separation machine; 15 . L type roller type transport platform; 16 . I type roller type transport platform; 17 . squeezing platform of the stamping machine; 18 . mechanical hand of the stamping machine; 19 . degumming and washing pool; 20 . chaining transport device; 21 . ramie fiber cleaning tank; 22 . trolley.
DETAILED DESCRIPTION OF THE INVENTION
[0038] The present invention adopts the apparatus shown in FIGS. 2 and 3 . This apparatus is an automatic degummed ramie production line used for separating the boon, bark and fiber layer of the ramie and degumming and fiber-separating, and washing and recovering the ramie fibers. In this production line, ramie is firstly sorted and transported by the sorting unit. The peeling unit peels off the bast fibers from the boon and collects the same separately to the ramie frame, namely the bast fiber collecting frame of the sequencing batch decorticator. The transport unit transports the ramie frame to the degumming unit for squeezing and degumming processing. The ramie fibers are then cleaned and recovered by the bast fiber cleaning unit.
[0039] The sorting unit is constituted by the ramie sorting platform 1 , which is located left to the automatic ramie stem separation machine 3 . The ramie sorting platform 1 can be the ramie sorting platform Model ZMFJ-1 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by sorting platform pivot, sorting platform driving mechanism, flat belt, and sorting platform stand.
[0040] The peeling unit is constituted by the sequencing batch decorticator 2 and three machines with the same structure, namely the automatic ramie stem separation machines 3 , wherein the sequencing batch decorticator is located the beginning end of the L type standing roller type transport platform 15 , followed immediately by the automatic ramie stem separation machine. The sequencing batch decorticator 2 can be the sequencing batch decorticator Model XBM-1D developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the bast fiber collecting frame of the sequencing batch decorticator 11 , the stem inlet of the sequencing batch decorticator 12 , the hoisting device, the rotating device, boon separating and recovering device, and the bast fiber cutting device. The automatic ramie stem separation machine 3 can be the automatic ramie stem separation machine Model ZDZMF-3 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the stem inlet of the automatic ramie stem separation machine 13 , the separation machine stand, the boon-and-bark separating device of the separation machine, and the bast fiber collecting and transporting mechanism. The L type standing roller type transport platform 23 can be the standing roller type transport platform Model GZSS-L developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the driving mechanism 21 , the roller 22 , and the stand 24 .
[0041] The transport unit is constituted by roller type transport platform 5 and chaining transport device 20 , wherein the roller type transport platform 5 is distributed right to the automatic ramie stem separation machine 3 and both front and rear sides of the stamping machine 6 , and the chaining transport device 20 is located over the degumming and washing pool 19 . The roller type transport platform 5 can be the roller type transport platform Model GZSS-1 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the driving mechanism, the roller, and the stand. The chaining transport device 35 can be the chaining transport device Model GLSS developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the stand, transport track, and the slidable hook.
[0042] The degumming unit is constituted by the degumming and washing pool 19 and four machines with the same structure, namely the stamping machine 6 , wherein the stamping machine 6 is located at the end of the roller type transport platform 5 , and the degumming and washing pool 31 is located 30 m away and right front of the stamping machine 6 . The degumming unit performs firstly the stamping machine squeezing processing in the degumming process, by which 80% of the gum can be removed, and then performs the degumming and washing processing. With the whole process, the degumming ratio can be up to 95% and the polluted wastewater caused by degumming can be reduced significantly. The stamping machine 6 can be the stamping machine Model XZMFX-3 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the stamping machine stand, the hydraulic motor, the squeezing platform of the stamping machine 17 , the mechanical hand of the stamping machine 18 , the squeezing and impacting device of the stamping machine.
[0043] The ramie frame convey unit is constituted by the first mechanical hand 4 and the second mechanical hand 7 , wherein the first mechanical hand 4 is located over the roller type transport platform 5 , fixed to the ground by the stand and across the L type standing roller type transport platform 23 . The second mechanical hand 7 is located at the rear of the roller type transport platform 5 and fixed to the ground by the stand.
[0044] The bast fiber cleaning unit is constituted by the third mechanical hand 9 two machines with the same structure, namely the ramie fiber back washing device 10 , wherein the third mechanical hand 9 is located left to the fiber back washing device and fixed to the ground by the stand. The bast fiber cleaning unit can clean up the residual chemicals on the ramie fibers in the ramie fiber cleaning process. At the same time, the process of performing batch washing can separate the residual boons in the ramie fibers by washing. The ramie fiber back washing device 10 can be the ramie fiber back washing device Model ZMXFC-1 developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, that is mainly constituted by the ramie fiber cleaning tank, the water supply device, the stand, and the cap inversing device. The soluble gum can be partially squeezed out from the ramie in the mechanical squeezing and water washing process to fiber-separating the raw fibers partially.
[0045] The ramie fiber back washing device 10 is located the very right side of the factory building and near the chaining transport device.
[0046] All of the first mechanical hand 4 , the second mechanical hand 7 , and the third mechanical hand 9 are the JXS-01 series mechanical hands developed jointly by Wuhan Textile University and Xinnong Ramie Co., Ltd, which are controlled using hydraulic system, and are steady, safe and reliable in working process.
[0047] In the apparatus of the present invention, the degumming and washing device 8 is right below the chaining transport device 20 in FIG. 7 .
[0048] In the apparatus of the present invention, the bast fiber collecting and transporting configuration of the automatic ramie stem separation machine 14 is at the right end of the automatic ramie stem separation machine 3 in FIG. 4 .
[0049] In the apparatus of the present invention, the I type roller type transport platform 16 is right over the L type roller type transport platform 15 in FIG. 5 .
[0050] In the apparatus of the present invention, the ramie fiber cleaning tank 21 is at the lower part of the ramie fiber back washing device 10 in FIG. 8 .
[0051] In the apparatus of the present invention, the trolley 22 is at the left part of the ramie fiber back washing device 10 in FIG. 8 .
[0052] The present invention will be further described below in combination with Examples and accompanied drawings, without limiting the present invention.
Example 1
[0053] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The manually peeled ramie marketed in Xianning City, Hubei Province was purchased. 500 kg of the manually peeled ramie was placed into the waste alkali bath pool in a bath ratio of 1:20 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0054] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0055] The manually peeled ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:20 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment. Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:20 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0056] Next, the manually peeled ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:20 (weight volume ratio), and immersed in a solution of 2 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:20 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0057] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 15 U (International units) in a bath ratio of 1:20 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0058] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 178, a BOD 5 of 33, a chromaticity of 11, a SS of 29, and a pH of 7.6. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0059] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
Example 2
[0060] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The manually peeled ramie marketed in Xianning City, Hubei Province was purchased. 500 kg of the manually peeled ramie was placed into the waste alkali bath pool in a bath ratio of 1:17 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0061] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0062] The manually peeled ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:17 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment. Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:17 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0063] Next, the manually peeled ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:17 (weight volume ratio), and immersed in a solution of 2.8 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:17 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0064] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 20 U (International units) in a bath ratio of 1:17 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0065] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 198, a BOD 5 of 40, a chromaticity of 15, a SS of 32, and a pH of 7.2. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0066] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
Example 3
[0067] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The manually peeled ramie marketed in Xianning City, Hubei Province was purchased. 500 kg of the manually peeled ramie was placed into the waste alkali bath pool in a bath ratio of 1:22 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0068] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0069] The manually peeled ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:22 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment. Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:22 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0070] Next, the manually peeled ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:22 (weight volume ratio), and immersed in a solution of 2.2 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:22 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0071] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 18 U (International units) in a bath ratio of 1:22 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0072] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 162, a BOD 5 of 37, a chromaticity of 17, a SS of 26, and a pH of 7.3. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0073] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
Example 4
[0074] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The fresh ramie in the Ramie Planting Field of Xianning City, Hubei Province was reaped. 500 kg of the fresh ramie was placed into the waste alkali bath pool in a bath ratio of 1:25 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0075] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0076] The ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:25 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment. Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:25 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0077] Next, the ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:25 (weight volume ratio), and immersed in a solution of 1.8 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:25 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0078] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 10 U (International units) in a bath ratio of 1:25 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0079] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 186, a BOD 5 of 39, a chromaticity of 12, a SS of 32, and a pH of 6.9. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0080] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
Example 5
[0081] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The manually peeled ramie originated in Yueyang City, Hunan Province was purchased. 500 kg of the manually peeled ramie was placed into the waste alkali bath pool in a bath ratio of 1:15 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0082] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0083] The manually peeled ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:15 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment. Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:15 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0084] Next, the manually peeled ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:15 (weight volume ratio), and immersed in a solution of 2.8 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:15 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0085] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 30 U (International units) in a bath ratio of 1:15 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0086] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 172, a BOD 5 of 36, a chromaticity of 15, a SS of 28, and a pH of 7.2. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0087] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
Example 6
[0088] The degumming processing was performed using the process flow shown in FIG. 1 and the apparatus shown in FIGS. 2 and 3 . The manually peeled ramie originated in Ruanjiang City, Hunan Province was purchased. 500 kg of the manually peeled ramie was placed into the waste alkali bath pool in a bath ratio of 1:18 (weight volume ratio) and immersed for 8 h. The solution in the pool was the alkaline wastewater discharged from the alkali-hydrogen peroxide one bath scouring-bleaching. Then, the degumming wastewater was precipitated by separate treatment, after which the resulted sludge was burnt directly and the supernatant was discharged into the sewage treatment unit.
[0089] The degumming wastewater was pumped into the sewage treatment unit, followed by the sewage treatment in the conditioning pool, the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool etc.
[0090] The manually peeled ramie treated in the waste alkali bath was placed into the anaerobic washing pool in a bath ratio of 1:18 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The anaerobic washing pool was circulated with the anaerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the anaerobic pool for sewage treatment.
[0091] Then, the manually peeled ramie treated in the anaerobic washing pool was placed into the aerobic washing pool in a bath ratio of 1:18 (weight volume ratio) and washed by immersion at ambient temperature for 8 h. The aerobic washing pool was circulated with the aerobic pool for sewage treatment, and the solution used for washing was with the same composition as that of the solution in the aerobic pool for sewage treatment. The aerobic washing pool was kept in the aerated state in the immersion period with the aerated dissolved oxygen of 3 to 5 mg/L.
[0092] Next, the manually peeled ramie treated in the aerobic washing pool was placed into the alkali-hydrogen peroxide one bath scouring-bleaching pool in a bath ratio of 1:18 (weight volume ratio), and immersed in a solution of 2.6 g/L NaOH and 0.5 g/L H 2 O 2 to react at the temperature of 80° C. for 2 h. The reaction liquid was discharged into the waste alkali bath pool. Then, the manually peeled ramie treated in the alkali-hydrogen peroxide one bath scouring-bleaching pool was placed into the fiber-separating and washing device in a bath ratio of 1:18 (weight volume ratio). The fiber-separating in the present invention can be performed either by rolling and rubbing manually or in a mechanical way. The washing time was 4 h.
[0093] Finally, the raw fibers treated by fiber-separating and washing were immersed in a solution with a cellulose concentration of 22 U (International units) in a bath ratio of 1:18 (weight volume ratio) and reacted at the temperature of 55° C. for 2 h so as to perform the bio-enzyme washing.
[0094] The effluents from the waste alkali bath, fiber-separating and washing, and bio-enzyme washing were pumped into the conditioning pool for sewage treatment, and treated in the anaerobic pool, the first precipitation pool, the aerobic pool, the second precipitation pool, after which the effluents had a COD of 182, a BOD 5 of 41, a chromaticity of 15, a SS of 35, and a pH of 7.4. The effluents were returned back to the fiber-separating and washing pool for repeated use.
[0095] The degummed ramie obtained after dehydration and baking was tested for fiber quality. The results were shown in Table 1.
[0000]
TABLE 1
Degummed Ramie Fiber Quality Test Results
Single Fiber
Metric
Fiber bundle
residual gum
Fineness
Number
breaking strength
content
Measurement
dtex
Nm
CN/dtex
%
units
National
≦8.33
≧1200
≧3.50
≦5.00
standard
Example 1
5.76
1680
4.50
3.82
Example 2
5.82
1750
4.21
4.17
Example 3
5.13
1720
4.46
4.08
Example 4
5.17
1810
4.39
3.42
Example 5
5.87
1670
4.40
4.12
Example 6
5.30
1851
4.42
4.38
[0096] As can be seen from Table 1, the degumming ramie fibers obtained by the degumming method provided in the present invention had relatively good qualities. The fiber linear density, the fiber bundle breaking strength, and the residual gum content met the national standard for degummed ramie (GB/T 20793-2006).
[0097] The ramie in the above examples may also be replaced by the ramie of other origins.
[0098] In the above examples, the degumming waste liquid after fiber-separating and washing and cellulose washing was pumped into the conditioning pool, in which the degumming wastewater had a COD of 1500 to 3000 significantly lower than the COD level of 8000 to 10000 in the conditioning pool of the traditional chemical degumming wastewater treatment system. The effluent from the second precipitation pool had a COD of not higher than 200, which can meet the requirements for water used in the fiber-separating and washing of the present process. After the treatment in conventional sewage treatment system, the effluent can reach the discharge standard B of Grade 1. | The present invention relates to a chain, continuous and no-waste method for degumming and fiber-separating the ramie, including anaerobic circle step, in which the raw fibers after the waste alkali bath step are immersed in the anaerobic water pool; aerobic circle step, in which the raw fibers after the anaerobic circle step are immersed in the aerobic water pool; alkali-hydrogen peroxide one bath scouring-bleaching step, in which the raw fibers after the aerobic circle step are immersed in a combined solution of NaOH and H 2 O 2 ; and the treatment by a fiber-separating and washing device followed by the immersion in the cellulase solution. In the present invention, the ramie degumming process and the degumming wastewater treatment are performed integratively, and the degumming wastewater is completely recycled after treatment. | 3 |
This application is a division of U.S. application Ser. No. 08/982,776, filed Dec. 7, 1997, now U.S. Pat. No. 6,196,659, issued Mar. 6, 2001, and claims priority under 35 U.S.C. § 119 to JP 323870, filed Dec. 4, 1996.
BACKGROUND OF THE INVENTION
“This application is a division of U.S. Application No. 08/982,776, filed Dec. 7, 1997, now U.S. Pat. No. 6,196,659, issued Mar. 6, 2001, and claims priority under 35 U.S.C. §119 to JP 323870, filed Dec. 4, 1996.”
1. Field of the Invention
The present invention relates to an ink jet recording apparatus capable of obtaining high quality images on a recording medium. More particularly, the invention relates to an ink jet recording apparatus that records by discharging recording ink and processing liquid such as an image enhancement agent that insolubilizes or coagulate coloring material in ink.
The present invention is applicable to all the equipment and devices that uses a recording medium formed by paper, cloth, leather, unwoven textile or the like, or a recording medium formed even by metallic material. As specific equipment and devices to which the present invention is applicable, there is a printer, a copying machine, a facsimile equipment, or some other office equipment or those usable as industrial production equipment.
2. Related Background Art
Conventionally, an ink jet recording method has been utilized for a printer, a copying machine, or the like, because this method enables operates at lower running costs with a lesser amount of noises, while making it easier to produce apparatuses compactly, and also, to facilitate color handling.
However, if it is intended to obtain images on a recording medium, which is the so-called ordinary paper, by means of those recording apparatuses that utilize the ink jet recording method, the waterproof capability of images thus recorded becomes insufficient or when it is intended to form color images, compatibility is not obtainable in forming highly densified images having no feathering and those having no running created between colors. As a result, it is impossible to obtain color images having good image fastness, and excellent quality as well.
In recent years, it has been made practicable to use the ink that contains waterproof coloring material in it as a method for enhancing the waterproof capability of recorded images. However, not only such waterproof capability is far from sufficient, but also, in principle, an ink of the kind is hardly soluble to water once it has been dried, which may often result in the nozzle clogging of a recording head. Therefore, there is apparently a disadvantage that the structure of the apparatus should become more complicated in order to prevent such nozzle clogging.
Also, a number of techniques have been disclosed conventionally for the enhancement of the fastness of recorded objects. In the specification of Japanese Patent Laid-Open Application No. 53-24486, a technique is disclosed, in which colors are laked and fixed by giving post-process to a colored object in order to promote wet fastness thereof.
In the specification of Japanese Patent Laid-Open Application No. 54-43733, a recording method is disclosed, in which the two or more components that promote the film formation capability when being in contact with each other at the room temperature or being heated by use of the ink jet recording method, thus making it possible to obtain a printed object whose film has been made strongly adhesive to the object when each of the components are in contact on a recording medium.
In the specification of Japanese Patent Laid-Open Application No. 55-150396, there is disclosed a method for providing water soluble color ink with the waterproofing agent for the formation of colors and lake after an ink jet recording has been executed.
In the specification of Japanese Patent Laid-Open Application No. 58-128862, an ink jet method is disclosed in which the position of an image to be recorded is discriminated beforehand, and then, recording ink and processing ink are overlaid for recording. A method is also disclosed in which a drawing is made in processing ink before recording ink is applied; processing ink is overlaid on a drawing written in recording ink beforehand; or recording ink is overlaid on a drawing written in processing ink beforehand, and processing ink is again overlaid to complete the drawing.
However, in these publications, no disclosure is made as to the recovery means, head structure, and tank structure, which are all characteristics of an ink jet recording apparatus for the maintenance of reliability of discharges, and also, as to the recording mode or the like which is needed for the enhancement of quality of recorded images.
On the other hand, there are fundamentally the problems inherent in the ink jet recording method as given below.
Firstly, ink adheres to the discharge opening surface of a recording head due to fine ink droplets (mist) generated other than the discharged main ink droplets when ink droplets are discharged from a recording head to a recording medium, such as a paper sheet, an OHP film, for recording, and ink droplets rebounded from the recording medium. If such ink is concentrated adhesively on the circumference of each discharge opening in a large quantity, or if paper particles or other foreign substances adhere to such concentration of ink, discharges are blocked, resulting in malfunction such as ink being discharged in the unexpected directions (twisting) or discharges of ink droplets being disabled (non-discharges).
Secondly, if ink in the nozzles of a recording head is evaporated and dried when printing is at rest, that is, if no discharges are made for a long time, to be exact, then overly viscous and fixed ink tends to clog the interior of nozzles to cause the twisted discharges or other defective discharges.
Therefore, in order to eliminate these unfavorable events, recovery means is provided for the ink jet recording method.
As means for cleaning and removing unwanted ink, paper particles and other foreign substances adhering to the discharge opening surface, which are caused by mist and rebounding ink droplets from a recording medium as described above as the first problem, it is generally adopted to arrange a structure in which the discharge opening surface is wiped off (wiping) by use of a blade formed by rubber or some other elastic material.
As means for solving the second problem described above, it is generally adopted to arrange the structure so that a recording head is capped to prevent ink from becoming overly viscous and fixed in the nozzle of the recording head at the time of non-recording, and that the ink, which becomes overly viscous and fixed to result in defective discharges and the adhesion of the foreign substances or the like and cannot be removed by means of the blade, is removed by exhausting the overly viscous ink from the nozzles by means of a suction pump connected with the cap for recovering the head for the performance of normal discharges. Further, for the operation of an on-demand type ink jet recording method, the plural discharge openings, which are arranged for one recording head, are not necessarily used at a time always. As a result, there are some nozzles that are not used for more than a certain period of time. Also, in a case where a plurality of recording heads are used such as for a color recording apparatus, there are some recording heads to which no data are transferred (the heads which are not currently engaged in recording), that is, the recording heads which are, not used. If a carriage is caused to scan or come to a stop while the discharge opening surface of the head mounted on it is not capped, ink is evaporated and dried on the discharge opening surface and in the interior thereof from which no ink has been discharged for a certain period continuously. As a result, the discharge capability is lowered to cause the degradation of recorded images eventually. In order to prevent such phenomenon as this, it is generally practiced for an ink jet recording apparatus to discharge ink in a specific location per certain periodical interval irrespective of recording data, thus causing ink in the nozzles to be exhausted to the outside to refresh ink. In this way, the discharge condition is always maintained normally and appropriately. Such ink discharge operation as this is called pre-discharge.
Ink by the pre-discharge described above is discharged to the location called pre-discharge position arranged separately in the cap of a recovery unit so that ink thus discharged is not caused to fly over a recording medium or in the interior of the recording apparatus to stain it.
For an ink jet recording apparatus that discharges ink and processing liquid, there is proposed a structure in the specification of Japanese Patent Laid-Open Application No. 8-281968 Japanese Patent Application No. 7-202635 in which caps, pumps, and wiping means are provided separately for use of ink discharge and for use of processing liquid discharge as a pre-discharge structure which is arranged for the solution of the problems described above.
Particularly, with regard to the wiping structure, it is proposed to provide a structure in which the wiping directions of ink and processing liquid are made different when wiping is performed in the main scanning direction of a carriage. However, this proposal is still insufficient from the viewpoint of the compatibility between a higher reliability such as no ink coagulation, fixation, or the like occurring in the recording apparatus and the simplification of the wiping mechanism.
Along the demands more on higher image quality, an ink jet recording apparatus has more numbers of nozzle arrays for discharging deep and light ink or the like. In this case, if a structure is still such as to wipe the nozzle arrays by the provision of the corresponding numbers of blades, it automatically leads to the increased costs inevitably.
SUMMARY OF THE INVENTION
It is one of the objects of the present invention to provide an ink jet recording apparatus capable of presenting excellent waterproof capability on an ordinary paper sheet in a better condition than the conventional art, and also, capable of presenting the compatibility between a highly reliable image recording that provides high quality having no feathering and running between colors at the time of color recording and a higher reliability with which it can prevent ink from being coagulated and fixed in the recording apparatus, hence preventing the head from being clogged.
It is another object of the invention to provide an ink jet recording apparatus capable of providing the compatibility between the higher reliability of preventing the coagulation and fixation of ink or the like in the recording apparatus and the simplification of the wiping mechanism therefor.
It is still another object of the invention to provide an ink jet recording apparatus comprising a carriage having a recording liquid discharge unit provided with recording liquid discharge openings for discharging recording liquid and a processing liquid discharge unit provided with processing liquid discharge openings for discharging processing liquid to process recording liquid arranged therefor to perform the movement thereof; wiping member for use of recording liquid dedicated to wiping the surface having the recording liquid discharge openings arranged therefor when the movement of the carriage is suspended; and wiping member for use of processing liquid dedicated to wiping the surface having the processing liquid discharge openings arranged therefor when the movement of the carriage is suspended. For this ink jet recording apparatus, the dedicated wiping by the wiping member for use of recording liquid and by the wiping member for use of processing liquid are executed, respectively, by changing the stopping position of the carriage.
In accordance with the preferred embodiments of the present invention, an ink jet recording apparatus is structured to discharge a recording medium beforehand a colorless or light colored liquid containing a chemical compound that insolubilizes coloring material in ink in accordance with image information, and then, to discharge monochrome color or multiple color ink in accordance with the image information. The apparatus thus structured is to perform wiping by moving wiping means for cleaning off the discharge opening surface of the ink jet recording head that discharges the processing liquid that insolubilizes coloring material in ink against solvent in the direction of the nozzle array of the ink jet head, and to make the stopping position of the carriage shiftable for wiping in accordance with the nozzle array of the ink jet head.
In accordance with the present invention, it is possible to materialize an ink jet recording apparatus for forming images by discharging ink and processing liquid to a recording medium, which is provided with a highly reliably recovery to produce good waterproof capability of images without running on the boundaries between different colors, but not to make coloring material in ink excessively insolubilized in the recording apparatus, with an arrangement that does not allow ink and processing liquid to be in contact with each other in the recovery system unit.
Particularly with respect to the wiping structure in which wiping is performed in the direction of increased nozzle arrays of an ink jet head, it is made possible to change the stopping positions of the carriage for the execution of wiping without increase the number of the blades, thus contributing to the reduction of costs significantly.
Also, the locus of the leading end of the wiping member is made parallel to the ink jet head when wiping is performed, thus facilitating the management and control of the amount of blade advancement and the contact angle and pressure to be exerted by the blade. Therefore, it becomes possible to enhance the performance of the blade.
Further, the wiping direction is made arbitrarily changeable in accordance with the nozzle array of an ink jet head. Also, the wiping member is provided with a first retracted position and a second retracted position where it does not abut upon the ink jet head so that the reciprocation of wiping becomes possible for the enhancement of wiping throughput accordingly.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view which shows the structure of the recording unit of an ink jet recording apparatus in accordance with the present invention.
FIG. 2 is an exploded perspective view which shows the structure of the carriage and the recording head and ink tank mountable on the carriage of an ink jet recording apparatus in accordance with the present invention.
FIG. 3 is an exploded perspective view which shows the structure of the recovery system unit of an ink jet recording apparatus in accordance with the present invention.
FIG. 4 is a cross-sectional view which shows the structure of the wiping mechanism of an ink jet recording apparatus in accordance with the present invention.
FIGS. 5A, 5 B and 5 C are views which illustrate the wiping operation in accordance with a first embodiment of the present invention.
FIGS. 6A, 6 B and 6 C are views which illustrate the wiping operation in accordance with a second embodiment of the present invention.
FIGS. 7A, 7 B and 7 C are views which illustrate the wiping operation in accordance with a fourth embodiment of the present invention.
FIG. 8 is a partially perspective view which shows the structure of the ink discharge unit of a recording head.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Hereinafter, with reference to the accompanying drawings, the specific description will be made of an ink jet recording apparatus in accordance with the present invention.
(Embodiment 1)
In FIG. 1 to FIG. 4, the ink jet recording apparatus of the present invention is shown.
In FIG. 1, a reference numeral 6 designates a carriage. On the carriage, the recording head 8 for normal use is mounted, having the processing liquid S nozzle array, the black ink BK nozzle array, and the color ink YMC nozzle array, which are arranged side by side, as well as the ink tanks 9 (see FIG. 5 A), such as the processing ink tank 9 S and color ink tanks 9 BK, 9 C, 9 M, and 9 Y, from the portion nearer to the printing region at the home position as shown in FIG. 2 . Each of the nozzle arrays of the color ink for yellow, magenta, and cyan is arranged side by side almost on the straight line.
Also, in FIG. 5C, a reference numeral 88 designates an optional recording head exchangeably mountable for use of the formation of images in higher quality, in which a processing liquid nozzle array, a black ink BK nozzle array, a light color ink YMC nozzle array and a deep color ink YMC nozzle array are arranged side by side.
The recording head 8 is electrically connected through a connector 6022 on the carriage 6 .
The recording head 8 is ink jet recording means that utilizes thermal energy for discharging ink, and provided with electrothermal transducing devices that generate thermal energy. Also, the recording head 8 utilizes changes of pressure exerted by the development and contraction of air bubbles formed by film boiling brought about by the application of thermal energy generated by the electrothermal transducing devices, hence discharging ink from the discharge openings for recording.
FIG. 8 is a partially perspective view which schematically shows the structure of the ink jet unit of the recording head 8 . In FIG. 8, a plurality of discharge openings 82 are arranged at specific pitches to form a nozzle array on the discharge opening formation surface 81 that faces a recording medium with a specific gap (approximately 0.5 to 2.0 mm, for example), and also, electrothermal transducing devices (heat generating resistors or the like) 85 are arranged along the wall surface of each of the liquid paths 84 conductively connected with a common liquid chamber 83 and each of the discharge openings 82 .
The recording head 8 is mounted on the carriage 6 with such a positional relationship that the discharge openings 82 are arranged in a direction intersecting the scanning (traveling) direction of the carriage 6 . In this state, the corresponding electrothermal transducing devices are driven (energized) in accordance with image signals or discharge signals to create film boiling in ink in each of the liquid paths 84 . The recording head 8 is structured to discharge ink from the discharge openings 82 by the application of the pressure thus exerted at that time.
Also, for the recording head 8 , ink supply openings 8030 are arranged (for use of processing liquid 8030 S, black 8030 BK, cyan 8030 C, magenta 8030 M, and yellow 8030 Y) for supplying ink from the processing liquid ink tank 9 S, color ink tanks 9 BK, 9 C, 9 M, and 9 Y respectively, and then, from the ink supply openings, ink is carried to each of nozzles of the recording head through the flow paths in the head accordingly.
As shown in FIG. 1, on both side walls of almost U-shaped chassis 1 , a guide shaft 4 and a supporting shaft 103 are arranged to slidably support the carriage 6 . The carriage 6 is driven by means of a carriage motor 104 through a driving belt 10 to reciprocate on these shafts in the scanning direction.
Also, a platen roller 2 and a pinch roller 3 are arranged to pinch and carry a recording medium (not shown) such as a paper sheet. The recording medium is carried on a platen 16 . At this juncture, the recording head unit (not shown) of the recording head mounted on the carriage 6 extrudes downward from the carriage 6 , while the discharge opening formation surface of the recording head unit faces the recording medium on the platen 16 in parallel to it. Here, the main body 40 to which the chassis 1 is fixed is provided with a waste ink tank 401 .
A recovery system unit 15 is arranged on the home position side, which is on the left-hand side of the ink jet recording apparatus in accordance with the present embodiment. FIG. 3 is a perspective view which shows the recovery system unit. Facing the recording head 8 , a processing liquid cap 113 , a black ink cap 12 , and color ink caps 114 and 115 are arranged from the right to the left in FIG. 3 .
In this respect, the processing liquid cap 113 and the black ink cap 112 serve dually as suction cap and untouched cap. The color ink caps 114 and 115 are dedicated to serving only as untouched caps, and then, the structure is made to suck color ink by use of the black ink cap 112 .
The caps 112 to 115 are fixed to the cap levers 131 to 133 , which are rotatively and axially fixed to the recovery system base 130 through the cap holder 122 to 125 , respectively. In this respect, the cap lever 131 serves dually to control cap holders 125 , 125 . The cap levers 131 to 133 are biased by cap springs. When a part of each of the levers slides on the cam surface 141 of the suction cam 140 , each of them rotates in the vertical direction. Here, the structure is arranged so that each of the caps 112 to 115 is made vertically movable along this rotation.
The processing liquid cap 113 and the black ink cap 112 of the recovery system unit 15 are conductively connected with the tubes 145 and 146 of the pump unit 119 through the cap holder 123 and 122 , respectively. The pump unit 119 is used for exerting negative pressure when the recording head presents defective discharges, which requires suction recovery or the like that sucks ink from the recording head while connecting the cap unit and the recording head. The pump unit 119 exemplified here is called a tube pump.
The pump unit 119 comprises tubes 145 and 146 ; a roller holder 144 , and a roller 147 . The roller holder 144 is rotatively and axially fixed to the recovery system base 130 . The tubes 145 and 146 are squeezed while the roller 147 , which is axially fixed to the roller holder 144 , pushes down the tubes 145 and 146 guided by the roller holder 144 , thus exerting negative pressure in the cap. The pump unit 119 is provided with the tube 145 which is dedicated to use of processing liquid, and the tube 146 for use of ink individually. Waste ink is carried to the waste ink tank by way of each individual path. This arrangement is needed for the prevention of insolubilization in the cap and pump, which may be caused if recording color ink and processing liquid are in contact with each other. Here, two systems of pump unit are shown for use of processing liquid and recording color ink. However, pump units may be provided for each of the caps individually.
The recovery system unit 15 is further provided with the processing liquid blade 117 that perform wiping for the discharge opening unit of the processing liquid recording head, and the color ink blade 118 that performs wiping for the discharge opening unit of the color ink recording head.
The processing liquid blade (first blade) 117 is arranged on the downstream side of the processing liquid nozzle array in the sheet conveying direction. The color ink blade (second blade) 118 is arranged on the downstream side of the black ink nozzle array in the sheet conveying direction. These blades are arranged each individually. Here, the color ink blade 118 moves in the arrangement direction of nozzle array, and as shown in FIGS. 5A, 5 B and 5 C, wiping is performed for the black and color nozzle arrays of the recording head for the normal use, and also, for the deep ink nozzle array of the recording head 88 for the optional use. A reference numeral 1119 designates the blade (third blade) that performs wiping for the light ink nozzle array of the recording head 88 for the optional use, which is arranged on the left side of the color ink blade 118 with a shift which is equivalent to the pitch portion of the nozzle array.
Each of these blades is formed by rubber or some other elastic material in order to wipe color ink or processing liquid adhering to each of the discharge opening formation surfaces of the recording heads.
As shown in FIG. 4, the blades 117 , 118 , and 1119 are fixed to the blade arm 142 installed movably on the guide unit 130 G of the recovery system base 130 in parallel to the recording head 8 . Also, the guide unit 130 G is arranged to control and manage the advancing amount of blade and its contact angle and pressure to keep them in normal condition constantly.
On a part of the blade arm 142 , the rack gear 142 G is arranged to engage with the driving gear 153 in a state of being biased by means of a wiper spring 152 . Each of the blades 117 , 118 , and 1119 is not allowed to be in contact with the recording head 8 when being biased by the wiper spring 152 (first retracted position A). Here, a reference numeral 130 S designates a device arranged for the recovery system base 130 to regulate the retracted position of the blade arm.
When the driving gear 153 is driven by means of a driving source to rotate, the blade arm 142 moves on the recovery system base 130 in parallel to the recording head 8 (forward). When the blades 117 , 118 , and 1119 move further from the position (second retracted position) where the blades do not abut upon the recording head after the blade arm 1423 has moved by the sufficient stroke of the nozzle array, the gear tooth of the driving gear 153 is partly cut off at 153 K. Therefore, the transmission of driving power is suspended, thus enabling the blade arm to return to the first retracted position by means of the spring force of the wiper spring 152 (backward).
In each of the blade arm retracted positions, the recording head 8 moves to an arbitrary position for the selection of the blades 117 , 118 , and 1119 . Then, reciprocal wiping becomes possible in the arbitrary direction.
FIGS. 5A, 5 B and 5 C are views which illustrate the wiping operation in accordance with the present embodiment.
FIG. 5A shows the initial position for wiping the nozzle array of the processing liquid S and the nozzle array of the black ink BK for the recording head 8 for normal use. FIG. 5B shows the initial position for wiping the nozzle array of the color ink YMC. FIG. 5C shows the initial position for wiping the nozzle array of the deep and light ink of the recording head 88 for the optional use.
In case of the recording head 8 for the normal use as shown in FIG. 5A, the blade is caused to move from the first retracted position to perform wiping in the forward direction for the processing liquid S nozzle array and the black ink BK nozzle array. Also, as shown in FIG. 5B, the recording head 8 is caused to move to the initial position for wiping the color ink YMC nozzle array, and the blade moves from the second retracted position to perform wiping in the backward direction for the color ink YMC nozzle array.
For the recording head 88 for the optional use, the blade is caused to move from the first retracted position, and as in the case shown in FIG. 5A, wiping is performed in the forward direction for the processing liquid S nozzle array and the black ink nozzle array. Also, as shown in FIG. 5C, the recording head 88 is caused to move from the second retracted position to the initial position for wiping the deep and light ink YMC nozzle arrays. The blade moves from the second retracted position to perform wiping in the backward direction for the deep and light ink YMC nozzle arrays, respectively.
(Embodiment 2)
FIGS. 6A, 6 B and 6 C are views which illustrate the wiping operation for an ink jet recording apparatus in accordance with another embodiment of the present invention. The mechanism of the ink jet recording apparatus of the present embodiment is the same as that of the first embodiment described in conjunction with FIGS. 1, 2 , 3 and 4 . Therefore, the description thereof will be omitted.
FIG. 6A shows the initial position for wiping the processing liquid nozzle array and the black ink BK nozzle array for the recording head 8 for the normal use. FIG. 6B shows the state that the recording head 8 is retracted to the position where no blade abuts upon the recording head 8 . The blade is caused to return from the second retracted position in the backward direction. FIG. 6C shows the initial position for wiping the color ink YMC nozzle array.
In accordance with the first embodiment, the wiping direction is changed depending on the nozzle arrays. The present embodiment is characterized in that the wiping directions of all the nozzle arrays are limited to one direction.
In other words, if the wiping direction for nozzle arrays should be defined only to the forward direction, the recording head 8 is retracted to the position where no blade abuts upon the recording head 8 , and then, the blade should be returned from the second retracted position in the backward direction after wiping.
Also, if the wiping direction for nozzle arrays should be defined only to the backward direction, the recording head 8 is retracted to the position where no blade abuts upon the recording head 8 , and then, the blade should be returned to the second retracted position, while the recording head 8 is caused to move to an arbitrary position. After that the wiping is performed.
(Embodiment 3)
FIGS. 7A, 7 B and 7 C are views which illustrate the wiping operation in accordance with still another embodiment of the present invention. The mechanism of the ink jet recording apparatus of the present embodiment is the same as that of the first embodiment described in conjunction with FIGS. 1, 2 , 3 and 4 . Therefore, the description thereof will be omitted.
FIG. 7A shows the initial position for wiping the processing liquid nozzle array and the black ink BK nozzle array of the recording head 8 for the normal use. FIG. 7B shows the initial position for wiping the color ink YMC nozzle array. FIG. 7C shows the initial position for wiping the deep and light ink nozzle arrays for the recording head 88 for the optional use.
The present embodiment is characterized in that the blade structure of the first embodiment is modified, that is, the second blade and the third blade are formed integrally for the reduction of the blade numbers in order to attempt the reduction of costs accordingly. | An ink jet recording apparatus with a carriage having a first liquid discharge unit with first liquid discharge openings and a second liquid discharge unit with second liquid discharge openings, the first liquid discharge unit and the second liquid discharge unit arranged for performing discharge when the carriage is moving, a first wiping member for wiping the first liquid discharge unit surface when the carriage is stopped at a first stopping position, and a second wiping member for wiping the second liquid discharge unit surface when the carriage is stopped at a second stopping position which is different from the first stopping position, wherein wiping by the first wiping member and the second wiping member is performed by movement of the respective wiping member along a direction different from the carriage movement direction. | 1 |
CLAIM OF PRIORITY
The present invention application claims priority from Japanese application JP 2006-105932 filed on Apr. 7, 2006 the content of which is hereby incorporated by reference into this application.
FIELD OF THE INVENTION
The present invention relates to a semiconductor optical modulation device and an integrated semiconductor light emission device integrating the same.
BACKGROUND OF THE INVENTION
With the proliferation of broad band networks, the trend of increasing the communication speed to 10 Gbit/s or higher has been accelerated in metropolitan optical communication networks connecting cities and relay stations. In the metropolitan optical communication networks, a fiber transmission distance of 40 to 80 km has been demanded for long distance transmission. In an optical communication system for the metropolitan optical communication network, it is an important subject to reduce the size and the power consumption of the optical transmitter/receiver module.
To reduce the size and the power consumption of the optical transmitter/receiver module, a system in which a temperature control mechanism for a light emission device is not required, i.e., an uncooled system is effective. For direct modulation systems for applying an electric signal directly to a semiconductor laser and generating a light signal, materials resistant to temperature changes have been selected, and heat dissipation of device structures has been improved. As disclosed in Non-Patent Document 1 (Optical Fiber Communication Conference 2003, PD40), for example, an uncooled high speed operation of 10 Gbit/s has been attained at an operation temperature of 100° C. or higher.
In the direct modulation system described above, however, the time fluctuation of a signal light wavelength (hereinafter referred to as chirping) is large in the high speed modulation operation at a modulation speed, for example, of 10 Gbit/s or higher. Thus, a 1300 nm band with small dispersion in optical fibers has been mainly used for the signal light wavelength band. In the signal light wavelength band of 1300 nm, however, the propagation loss in the optical fiber is large. This is not suitable for long distance transmission of 30 km or more.
Generally, to transmit a high speed light signal at a modulation rate of 10 Gbit/s or more for 40 km or more, an external modulation system in which only small chirping is generated is used. Particularly, a semiconductor electro-absorption (EA) modulation device utilizing the electro-absorption effect has excellent features with respect to reduction in size, power consumption, integration ability with a semiconductor laser, etc. Particularly, a semiconductor optical integrated device in which the EA modulation device and a distributed feedback (DFB) semiconductor laser with an excellent single-wavelength property are monolithically integrated on one semiconductor substrate (hereinafter referred to as EA/DFB laser) has been used generally as a long distance transmitting light emission device for transmission over the distance of 40 km or more. In this case, the signal light wavelength of a 1550 nm band with a small transmission loss of optical fibers has been mainly used.
In order to decrease the size and the power consumption of the optical communication module for the metropolitan optical communication network, it is desirable that the EA/DFB laser be uncooled in a similar manner to the direct modulation system. For the conventional EA/DFB laser, however, a temperature control function is required for the normal operation, and an uncooled operation is impossible. The reason will be described with the operation principle of the EA modulation device.
For the normal operation of the EA/DFB laser, it is important to appropriately set a detuning (λ signal −λ EA ) defined as a difference between a signal light wavelength λ signal of the laser and a gain peak wavelength λ EA of the EA modulation device. In a state where a voltage is not applied to the EA modulation device, the optical absorption edge wavelength of the EA modulation device is sufficiently separated from the signal light wavelength so that an optical absorption does not occur. That is, the EA modulation device is transparent to the signal light. In this case, the signal light permeates the EA modulation device and is in an ON state as the optical output. When a voltage is applied to the EA modulation device, on the other hand, the optical absorption edge wavelength of the EA modulation device shifts toward the long wavelength side through the Franz-Keldysh effect or the quantum confine Stark effect to overlap with the signal light wavelength. In this case, the signal light is absorbed to the EA modulation device and the optical output is in an OFF state.
The light intensity ratio of the ON state and the OFF state of the signal light passing through the EA modulation device and flowing out is referred to as an extinction ratio. The larger the extinction ratio is, the more it is preferred for signal transmission without an error. A high speed light signal can be generated by modulating the voltage applied to the EA modulation device at a high speed.
In the operation principle of the EA modulation device, if the detuning is excessively small, the optical absorption edge wavelength of the EA modulation device is always overlapped with the signal light wavelength. As a result, the insertion loss increases due to the increase in the fundamental absorption, whereby a sufficient optical output cannot be obtained in the ON state of the light signal to increase the bit error rate after transmission. On the other hand, in the case where the detuning is excessively large, an application voltage increases, which is required till the optical absorption edge wavelength of the EA modulation device is overlapped with the signal light wavelength. This is not suitable for a low power consumption operation. Further, in the case where the voltage applied to the FA modulation device is excessively high, wave functions of carriers leak from the quantum well, resulting in a problem of deteriorating the extinction ratio.
The detuning in the EA/DFB laser needs to be set such that the signal light is not absorbed in the ON state in which the electric field is not applied, and extinction can be sufficiently attained within a practical range of the voltage in the OFF state in which the signal light is absorbed.
On the other hand, the light emission device is demanded to normally operate at an operation temperature between −5° C. and 85° C., the light emission device being used for an optical communication module for small, low consumption power communications for the metropolitan optical communication network. However, the detuning of the EA modulation device largely varies depending on the operation temperature. This will be described with reference to FIG. 1 .
FIG. 1 shows the temperature dependence of the gain peak wavelength λ EA in an extent EA modulation device with a broken line and the temperature dependence of the oscillation λ signal in DFB laser with a solid line. The temperature dependence of λ EA is related to the temperature dependence of the semiconductor band gap which is about +0.65 nm/° C. On the other hand, the temperature dependence of λ signal is related to the temperature dependence of the diffraction grating, which is about +0.1 nm/° C. Thus, the temperature dependence of the change of the detuning as the difference between them is about +0.55 nm/° C., and the detuning changes by about 50 nm upon the temperature change from −5° C. to 85° C. In the conventional EA/DFB laser, the fluctuation range for the detuning in which the normal operation is possible is about ±5 nm, and temperature control is applied so as to provide a predetermined characteristic, for example, at a temperature of 25° C.
Since the detuning of the EA/DFB laser, as described above, changes as much as about 50 nm, it greatly exceeds ±5 nm, which is the fluctuation range for the detuning in which the normal operation is possible. The optical loss increases at high temperature, making it difficult for ensuring the intensity of light sufficient for long distance transmission.
For solving the problem of the change of the detuning by temperature described above and attaining the uncooled system for the ED/DFB laser, the EA modulation device is set as shown by a dotted chain λ′ EA in FIG. 1 such that the detuning has an appropriate value at an estimated highest working temperature, for example, at a temperature of 85° C. At a working temperature lower than the estimated highest working temperature, it is possible to adopt a method of applying an offset bias V OH to EA modulation device in accordance with the temperature change, thereby shifting the optical absorption edge wavelength of the EA modulation device and controlling it so as to always keep an appropriate detuning even when the working temperature changes. Known examples of the uncooled EA/DFB using the method include, for example, those described in Non-Patent Document 2 (Optical Fiber Communication conference 2003, PD 42) or Non-Patent Document 3 (30 th ECOC 2004, Mo 4.4.7).
In the Non-Patent Documents 2, 3, a signal light wavelength in a 1300 nm band is used. In the signal light wavelength in the 1300 nm band, the optical loss is large during transmission through an optical fiber. It is not suitable for long distance transmission for a distance of 20 km or more. For long distance transmission for a distance of 40 km or more necessary for the metropolitan optical communication network, it is desirable that the operation be possible in the 1550 nm band of the signal light wavelength with a small optical loss during fiber transmission. Known examples for an uncooled EA/DFB in the 1550 nm band suitable for a long distance communication include, for example, those described in Non-Patent Document 4 (Electronics Letters, 2003, Vol. 39, No. 259), or Non-Patent Document 5 (Optical Fiber Communication Conference 2004, ThD4).
In the Non-Patent Document 4, there is no specific description about detuning and about a semiconductor quantum well structure as an optical absorption layer. Further, the Non-Patent Document 5 discloses detuning of 55 nm at a temperature of 25° C. This is a value substantially identical with that in the existent EA/DFB laser. This value does not correspond to detuning suitable for the 1550 nm band which is preferred for the long distance communication proposed in the present invention.
[Non-Patent Document 1]: Optical Fiber Communication Conference 2003, PD40
[Non-Patent Document 2]: Optical Fiber Communication Conference 2003, PD44
[Non-Patent Document 3]: 30th ECOC 2004, Mo 4.4.7
[Non-Patent Document 4]: Electronics Letters, 2003, Vol. 39, No. 25
[Non-Patent Document 5]: Optical Fiber Communication Conference 2004, ThD4
SUMMARY OF THE INVENTION
The present invention provides a light emission device using an EA modulator having optimal detuning in the 1550 nm band and a quantum well structure suitable for a long distance optical communication for a distance of 40 km or more, thereby providing an inexpensive light source.
For the operation of the EA/DFB laser in the 1550 nm band of the signal light wavelength, trade off between the chirping and the extinction ratio needs to be considered. This is because the amount of the dispersion during fiber transmission in the 1300 nm band of the signal light wavelength is substantially zero, while the fiber dispersion is as large as about 20 ps/nm/km in the 1550 nm band. For the setting of the detuning assuming the uncooled operation, when the temperature becomes lower, the detuning becomes larger. The larger detuning is, the higher voltage is required for controlling the detuning to an appropriate detuning. In this case, the slanting of the band increases to decrease the confinement effect of carriers in the quantum well. As a result, a spatial overlap of the wave functions of electrons and holes is decreased to deteriorate the extinction ratio.
For ensuring the extinction ratio during an uncooled operation, it is necessary to strongly confine electrons with a small effective mass in the quantum well. For this purpose, it is effective to use, for example, a method of decreasing the well width of the quantum well to enhance the quantum effect or a method of increasing the difference between the composition wavelengths of the quantum well layer and the barrier layer to increase the energy band offset between both of them. However, using the methods described above means to increase chirping. The methods are not suitable for the operation in the 1550 nm band of the signal light wavelength.
In the conventional EA/DFB laser, a multi-quantum well at least including In, Ga, As, and P is generally used as the optical absorption layer. In the InGaAsP system quantum well described above, the trade off between the chirping and the extinction ratio is severe, as described above. The long distance transmission for a distance of 40 km or more by the uncooled operation is difficult to be attained. This is due to the feature in which, in the band structure of the InGaAsP material system, the energy band offset between the quantum well layer and the barrier layer is smaller on the side of the conduction band and larger on the side of the valance band. On the contrary, the quantum well structure in which the well layer is made of InGaAlAs, InGaAsP, or InGaAs, and the barrier layer is made of InGaAlAs or InAlAs has excellent features as described below and can be said suitable as an optical absorption layer of the EA modulation device aiming at an uncooled operation.
(1) The band offset on the side of the conduction band is large and the leakage of the wave function to the outside of the quantum well is small in the quantum well structure. Thus, a spatial overlap of wave functions of electrons and holes is large, and the extinction ratio is improved. (2) The energy band offset between the quantum well and the barrier layer is smaller on the side of the valence band than on the side of the conduction band. Holes are hardly accumulated in the quantum well. Thus, since this is suitable for a high speed modulation operation and chirping during modulation is suppressed, this is advantageous for long distance transmission.
The inventors of the present application have experimentally proved that fiber transmission for a distance of 40 km at a modulation speed of 10 Gbit/s by an uncooled operation is possible by applying an InGaAlAs system material to the EA modulation device and setting an appropriate detuning in the EA/DFB laser aiming for the uncooled operation.
As has been described above, for the normal operation of the EA/DFB laser, it is important to set appropriate detuning. Setting of detuning suitable for the uncooled EA/DFB laser is described with reference to FIG. 2 .
The abscissa shown in FIG. 2 represents detuning at a temperature of 25° C. The ordinate on the left represents an insertion loss based on the fundamental absorption edge wavelength at a temperature of 85° C. which is an upper limit for the assumed operation temperature. The ordinate on the right represents an extinction ratio at −5° C. which is a lower limit for the operation temperature. As the detuning at a temperature of 25° C. decreases, the insertion loss based on the fundamental absorption edge wavelength at a temperature of 85° C. which is the upper limit for the operation temperature increases. This is because detuning decreases at a temperature of 85° C. (refer to FIG. 1 ). When the detuning at a temperature of 25° C. decreases to 80 nm or less, the insertion loss based on the fundamental absorption edge wavelength at a temperature of 85° C. exceeds 5 dB. In principle, the EA modulation device has a modulation loss which is a loss during modulation, as well as the insertion loss. It is difficult to suppress the modulation loss to the value of 4 dB or less. In the case where the sum of the insertion loss and the modulation loss at a temperature of 85° C. is 9 dB or more, it requires a large current for the DFB laser in order to obtain an optical output during modulation, the optical output being necessary for performing long distance transmission for a distance of 40 km or more without a relay, which is not suitable for the operation at low power consumption. Thus, it is desirable to set the detuning at a temperature of 25° C. of the uncooled EA/DFB laser to 80 nm or more.
On the other hand, taking notice on the extinction ratio at −5° C. which is a lower limit of the operation temperature, the larger the detuning at a temperature of 25° C. of the EA/DFB laser, the lower the extinction ratio at −5° C. is. This is because detuning at −5° C. increases excessively (refer to FIG. 1 ). When the detuning at a temperature of 25° C. exceeds 120 nm, extinction ratio at −5° C. is reduced to less than 10 dB. Generally, for signal transmission without a signal error, 10 dB or more is necessary for the dynamic extinction ratio as an extinction ratio during high speed modulation. For this purpose, when considering the extinction ratio at a low temperature, it is desirable that detuning at a temperature of 25° C. be 120 nm or less.
From the experimental perspective described above, it is preferred that the detuning at a temperature of 25° C. suitable for the uncooled operation of the EA/DFB laser be preferably set between 80 nm and 120 nm. More generally, the following expression is shown by using the energy E signal corresponding to the signal light wavelength at a temperature of 25° C. and the energy E EA corresponding to the gain peak wavelength of the EA modulation device at a temperature of 25° C.: 40 meV<(E EA −E signal )<70 meV
FIG. 3 shows an optimal range of the detuning proposed by the invention in the case where the signal light wavelength at a room temperature (25° C.) is 1500 nm. In the case where the signal light wavelength at the room temperature is 1550 nm, the optimal gain peak wavelength of the EA modulation device according to the proposal of the invention is between 1430 nm and 1470 nm. This corresponds to a region shown by hatched lines in the figure. The signal light wavelength is not applied only to 1550 nm. Even in the case where the signal light wavelength is one of the values between 1450 nm and 1630 nm, the same relation as hereinabove described is established with respect to the detuning setting. In this case, the gain peak wavelength of the EA modulation device may be set to the value from 1340 nm to 1550 nm while considering the optimal detuning.
It has also been studied on the range of a composition wavelength suitable for the barrier layer in the quantum well structure at a temperature of 25° C., the barrier layer being used as an absorption layer of the EA modulation device of the uncooled EA/DFB laser, with respect to the trade off between the optical loss and the chirping at a high temperature. As shown in FIG. 4 , the abscissa represents a compositional ratio of the barrier layer at a temperature of 25° C. FIG. 4 is based on the experimental data using an EA/DFB laser at the signal light wavelength of 1550 nm, and the gain peak wavelength of 1470 nm of the EA modulation device at a temperature of 25° C. The ordinate on the left represents a contribution to the insertion loss due to the optical absorption of the barrier layer at a temperature of 85° C. The ordinate on the right shows the energy band offset on the side of the valence band (hereinafter referred to as ΔEv) between the quantum well and the barrier layer.
As shown in FIG. 4 , as the composition wavelength of the barrier layer at a temperature of 25° C. is longer, the contribution to the insertion loss due to the optical absorption effect of the barrier layer at a temperature of 85° C. increases. This is because that the composition wavelength of the barrier layer at a temperature of 85° C. becomes longer than the composition wavelength of the barrier layer at a temperature of 25° C. and approaches to the signal light wavelength due to the decrease in the band gap with the increase of the temperature. Further, as shown in FIG. 4 , when the composition wavelength of the barrier layer at a temperature of 25° C. exceeds 1350 nm, the contribution to the insertion loss due to the optical absorption of the barrier layer at a temperature of 85° C. exceeds 3 dB. In this case, it is difficult to suppress the sum of the insertion loss and the modulation loss in the EA modulation device to the value of 9 dB or less. As a result, a large current is required for the DFB laser in order to obtain an optical output upon modulation necessary for performing long distance transmission for 40 km or more without a relay. This is not suitable for a low power consumption operation. Thus, the composition wavelength of the barrier layer at a temperature of 25° C. is preferably 1350 nm or less. More generally, the following expression is shown by using the energy E signal corresponding to the signal light wavelength and the energy E barrier corresponding to the compositional ratio of the barrier layer: (E signal +120 meV)<(E barrier )
On the other hand, as the composition wavelength of the barrier layer at a temperature of 25° C. is shortened, the value of ΔEv increases. As ΔEv increases, a plurality of quantum levels are formed in the quantum well on the side of the valence band to increase the ratio of the fluctuation of the refractive index relative to the fluctuation of the carrier density. As a result, chirping increases so that this is not suitable for long distance transmission for a distance of 40 km or more. In order to suppress the chirping, it is desirable to decrease ΔEv as small as possible. In a state where a constant temperature is set, the EA modulation device uses the quantum well as the optical absorption layer, the quantum well including an InGaAsP system material, which attains the long distance transmission for a distance of 40 km at 10 Gbit/s. In the EA modulation layer, ΔEv is about 120 meV. In the quantum well structure made of the InGaAlAs system material, when ΔEv is set to 120 meV, the wavelength of the barrier layer at a temperature of 25° C. is 1050 nm relative to the gain peak wavelength of 1470 nm of the EA modulation device at a temperature of 25° C. Thus, it is desirable to set the compositional ratio of the barrier layer to 1050 nm or more when the gain peak wavelength of the EA modulation device at a temperature of 25° C. is 1470 nm, in the EA modulation device using the InGaAlAs system quantum well as the optical absorption layer. More generally, the following expression is shown by using the energy E EA corresponding to the gain peak wavelength of the EA modulation device at a temperature of 25° C. and the energy E barrier corresponding to the barrier composition wavelength at a temperature of 25° C.: E barrier <(E EA +350 meV)
From the consideration described above, as the setting for the quantum well barrier layer suitable for the uncooled operation of the EA/DFB laser aiming at long distance transmission for a distance of 40 km or more, it is preferably expressed below:
( E signal +120 meV)< E barrier <( E EA +350 meV)
The signal light wavelength is not restricted to 1550 nm. However, even if the signal light wavelength is one of the values between 1450 nm and 1630 nm, the setting of composition wavelength of the barrier layer in the quantum well structure of the EA modulation device suitable for the uncooled operation of the EA/DFB laser, it can be easily estimated the same relation as hereinabove described is established.
In the experimental study described above, while the DFB laser is used as a light source for supplying a signal light to the EA modulation device, it may not necessarily be restricted to the DFB laser but a similar effect can be obtained also by a distributed Bragg reflector (DBR). Additionally, it is not always necessary that the EA modulation device and the light source for supplying the signal light are monolithically integrated. Also, in the case of using an external light source constituted so as to condense the signal light to the EA modulation device by using some means, a relation between the signal light wavelength and the detuning and the relation between the signal light and the barrier layer composition wavelength do not essentially change.
Further, in the above discussion, the uncooled operation of the EA/DFB laser is noted. In the case of using a variable wavelength light source capable of changing the wavelength of the signal light by some means as the light source for supplying the signal light, the relation between the signal light wavelength and the detuning or the relation between the signal light wavelength and the barrier layer composition wavelength do not essentially change.
There is a problem of the change of the detuning due to the change of temperature in the uncooled operation. However, in the case of using the variable wavelength laser for the light source supplying the signal light, the gain peak wavelength of the EA modulation device does not change. The detuning changes due to the change of the signal light wavelength. The longest oscillation wavelength of the variable wavelength laser is λ signal . The gain peak wavelength of the EA modulation device at the operation temperature is λ EA . With consideration of the trade off between the insertion loss during the operation of shortest wavelength of the variable wavelength laser and the extinction ratio during the operation of the longest wavelength, It can be easily considered that the following expression is desirable in the same manner as in the uncooled operation:
40 meV<( E EA −E signal )<70 meV
( E signal +120 meV)< E barrier <( E EA +350 meV)
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing an embodiment of the temperature dependence of the gain peak wavelength λ EA of the EA modulation device and the oscillation wavelength λ signal of the DFB laser.
FIG. 2 is a graph showing the dependence of the insertion loss based on the fundamental absorption edge wavelength at a temperature of 85° C. which is the upper limit of the operation temperature ( FIG. 2A ), and the detuning corresponding to the extinction ratio at a temperature of −5° C. which is the lower limit of the operation temperature in the EA/DFB laser ( FIG. 2B ).
FIG. 3 is a graph showing an embodiment of an optimal range of the gain peak wavelength of the EA modulation device corresponding to a signal light wavelength of a DFB laser proposed in the present invention.
FIG. 4 is a graph showing an embodiment of the dependence of the contribution to the insertion loss based on the optical absorption of a barrier layer at a temperature of 85° C. which is an upper limit of an operation temperature of a quantum well structure used as an absorption layer of an EA modulation device ( FIG. 4A ) and the composition wavelength of the barrier layer at a temperature of 25° C. with an energy band offset on the side of the valence band between the quantum well and the barrier layer in the EA/DFB laser ( FIG. 4B ).
FIG. 5 is a view showing a former-half for the manufacturing step of a semiconductor optical integrated device according to Embodiment 1 of the present invention.
FIG. 6 is a view showing a latter-half for the manufacturing step of a semiconductor optical integrated device according to Embodiment 1 of the invention.
FIG. 7A is a perspective view for the constitution of a semiconductor optical integrated device as a BH structure according to Embodiment 2 of the invention. FIG. 7B is a perspective view showing a cross section thereof cut along a central line.
FIG. 8A is a perspective view for the constitution of a semiconductor optical integrated device as a variable wavelength LD according to Embodiment 3 of the present invention. FIG. 8B is a perspective view showing a cross section thereof cut along a central line.
FIG. 9 is a schematic view showing the outline of a structure for an embodiment of a transmission/receiving module using the semiconductor optical integrated device described in Embodiment 1 and Embodiment 2.
FIG. 10 is a schematic view showing the outline of a control system for an embodiment of a transmission/receiving module using the semiconductor optical integrated device described in Embodiment 1 and Embodiment 2, which is a schematic view showing a fifth embodiment of the present invention.
FIG. 11 is a schematic view showing a terminal of an optical communication system constituted by an optical transmitter/receiver package in which an optical transmission module of the present invention shown in FIG. 9 and FIG. 10 , and an optical receiving module separately assembled are mounted.
DESCRIPTION OF THE PREFERRED EMBODIMENT
According to the present invention, a semiconductor optical modulation device suitable for the uncooled operation can be realized. Further, by using the optical modulation device according to the present invention, a light emission device does not require a mechanism for controlling a device temperature due to integration with a single mode laser such as a DFB laser or DBR laser. The light emission device suitable for long distance transmission for a distance of 40 km or more can be manufactured at a low cost. Further, an optical device integrating with an optical modulation device, which supports a wide variable wavelength, can be attained by integration with a variable wavelength light source.
Embodiment 1
RWG-EA/DFB (DBR)
A process for manufacturing a semiconductor optical integrated device according to Embodiment 1 of the present invention is described with reference to FIG. 5 and FIG. 6 . The drawings are only for the purpose of explaining the embodiment. The size and scale of the drawings showing the embodiment are not necessarily identical.
At first, a quantum well structure 2 made of an InGaAlAs system is formed on an n-InP substrate 1 as an electro-absorption optical modulator using an MOCVD method ( FIG. 5A ). In this case, a light emission wavelength of the quantum well structure at a temperature of 25° C. is about 1470 nm. For example, a desired light emission wavelength can be obtained by laminating a quantum well layer with a thickness of 6 nm and with a compositional ratio of In, Ga, and Al at 0.54:0.38:0.08, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.52:0.33:0.15. Further, an optical confinement structure sufficient for extinction can be formed as the quantum well structure by alternately laminating about 10 layers of the quantum wells and the barrier layers. Then, etching is performed up to the surface of the n-InP substrate 1 while leaving the electro-absorption optical modulator of a desired length ( FIG. 5B ). The etching technique for the semiconductor layer having In, Ga, Al, and As is described in detail, for example, in JP-A No. 2005-150181.
Then, a quantum well structure 3 made of an InGaAlAs system is formed as a semiconductor laser portion ( FIG. 5C ). The light emission wavelength of the quantum well structure 3 at a temperature of 25° C. is about 1540 nm. For example, a desired light emission wavelength can be obtained by laminating a quantum well layer with a thickness of 4 nm and with a compositional ratio of In, Ga, and Al at 0.65:0.3:0.05, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.55:0.33:0.12.
Further, an optical confinement structure suitable for laser oscillation can be formed by alternately laminating about 8 layers of the quantum wells and the barrier layers. Although not illustrated, a carrier confinement structure suitable for laser oscillation can be formed by sandwiching the quantum well structure 3 between InAlAs bulk grown layers with a thickness of about 100 nm and with a compositional ratio of In and Al at 0.52:0.48.
Then, etching is performed up to the surface of the n-InP substrate 1 while leaving a semiconductor laser portion of a desired length so as not to influence the electro-absorption optical modulator described above. The etching technique is disclosed specifically in JP-A No. 2005-150181 as described above.
Then, an optical waveguide layer 4 made of an InGaAsP system is formed between the electro-absorption optical modulator and the semiconductor laser portion described above ( FIG. 5D ). As a detailed structure of the optical waveguide layer 4 , for example, the following structure is desirable: an InGaAsP bulk growth layer with a thickness of 100 nm and with the composition wavelength of 1150 nm is formed, an InGaAsP growth layer with a thickness of 200 nm and with the composition wavelength of 1300 nm, and an InGaAsP bulk growth layer with a thickness of 100 nm and with the composition wavelength of 1150 nm are successively formed. An optical waveguide layer with a small optical loss can be formed by the structure described above.
Then, a diffraction grating 5 is formed by etching on the quantum well structure 3 made of the InGaAlAs system as the semiconductor laser portion ( FIG. 5E ). As the diffraction grating layer, a semiconductor having a higher refractive index than that of InP is desired. For example, an InGaAsP growth layer with a thickness of 30 nm and with the composition wavelength of 1150 nm is preferred. In order to form the diffraction grating, a pattern formation to a resist using either a holographic exposure method or an electron beam drawing method, both of which are known techniques, and either of a wet or dry etching step may be combined. As a specific resist pattern, stripes at a pitch of about 240 nm may be formed in the direction perpendicular to mesa. This can provide a stable longitudinal single mode oscillation suitable for optical communications.
Then, a part of the side of a light emission edge of the quantum well structure 2 made of the InGaAlAs system, which is formed as the electro-absorption optical modulator described above, is etched to reach the n-InP substrate 1 , forming a window structure 6 ( FIG. 5F ).
Successively, a p-InP layer 7 is formed by an MOCVD method ( FIG. 6A ). Then, except for the portion forming the ridged waveguide, the p-InP layer 7 is etched up to the surfaces of the quantum well structure 2 , the quantum well structure 3 and the optical waveguide layer 4 in order to form a ridged waveguide structure 13 . The quantum well structure 2 made of the InGaAlAs system is formed as the electro-absorption optical modulator. The quantum well structure 3 made of the InGaAlAs system is formed as the semiconductor laser portion ( FIG. 6B ). In this case, a stable transverse single mode oscillation suitable for optical communications can be obtained by forming the ridge with a width of about 2 μm.
Then, after forming a silicon oxide film 8 on the entire surface by a thermal CVD method ( FIG. 6C ), the silicon oxide film 8 is removed only from the top surface of the ridged portion 13 of the semiconductor light emission device and the electro-absorption optical modulator. While the silicon oxide film is used in this embodiment, a silicon nitride film or the like may also be used instead. Then, the wafer is planarized by a polyimide resin 9 in plane with the top surface of the ridged portion 13 on which the silicon oxide film 8 is removed. Then, a p-electrode 10 for the optical modulator and a p-electrode 11 for the semiconductor laser portion are formed. As the electrode materials, known Ti and Au may be successively formed.
Successively, an n-electrode 12 is formed at the rear face of the n-InP substrate 1 . As the electrode materials, known AuGe, Ti, and Au may be successively formed in the same manner described above ( FIG. 6D ).
After forming the electrode, the device is cut out by cleavage. A reflection film with reflectivity of 90% is formed at the rear end surface and a low reflection film with reflectivity of 1% or less is formed at the front end surface by a sputtering method.
According to the method described above, a ridged waveguide type semiconductor optical integrated device in which the EA modulator portion and the DFB laser portion are integrated on one identical substrate can be formed. The order of crystal growth of the EA modulation portion, the waveguide portion, and the DFB laser portion is not limited to this. For example, In the case of forming the DFB laser portion at first, the device structure obtained does not change. With respect to the material for the electro-absorption optical modulator, a quantum well structure may be used, in which the well layer is made of any one of InGaAlAs, InGaAsP, and InGaAs, and the barrier layer is made of either one of InGaAlAs or InAlAs. As the material for the semiconductor laser portion, an InGaAsP system may be used instead of the InGaAlAs system. As the material for the optical waveguide, an InGaAlAs system may be used instead of the InGaAsP system.
The method of crystal growth is not necessarily limited to the MOCVD method and may be formed, for example, using an MBE method. Further, the EA modulation portion, the waveguide portion, and the DFB laser portion may be formed by a single process of the crystal growth by using a selective area growth method. Further, a bent waveguide structure may be used instead of the window structure. Planarization by using the polyimide is not always necessary.
Based on the procedures described above, a method of manufacturing a device in the case where the DFB laser portion is replaced with a structure having other optical functions such as a DBR laser or a SOA can be easily inferred.
Then, an operation method of the ridged waveguide type semiconductor optical integrated device of Embodiment 1 is described. Laser oscillation is obtained by applying a forward bias to the p-electrode 11 of the semiconductor laser portion. In this case, since light is periodically fed back by the diffraction grating 5 , the oscillation spectrum is a single mode and the oscillation wavelength is 1550 nm. The laser light passes the optical waveguide 4 and enters the electro-absorption optical modulation portion 2 . The laser light is absorbed by applying a reverse bias to the p-electrode 10 of the optical modulation portion. This allows the light to be turned ON and OFF. After light laser passes the electro-absorption optical modulation portion 2 , the light laser passes the window structure 6 and goes out to the outside of the device. This can facilitate optical coupling with an optical fiber and suppress the coupling loss to the value of 3 dB or less. The operation current of the semiconductor laser portion was within a range from 70 to 150 mA at a temperature of −5° C. to 85° C. Further, by optimally controlling the voltage applied to the electrode 10 for modulation in accordance with the peripheral temperature of the ridged waveguide type semiconductor optical integrated device of Embodiment 1, a dynamic extinction ratio of 10 dB or more was obtained during the operation at a modulation rate of 10 Gbps. As a result, a favorable eye opening for a transmission distance of 40 km or more at a bit rate of 10 Gbps at a temperature of −5° C. to 85° C. without controlling the temperature was available.
Embodiment 2
BH-EA/DFB (DBR)
FIG. 7A is a perspective view illustrating a construction according to another embodiment of a semiconductor optical integrated device applied with the present invention. FIG. 7B is a perspective view illustrating a cross section cut along a central line. However, the drawing is only for explaining this embodiment and the size and scale of the drawing showing this embodiment are not necessarily identical.
At first, a quantum well structure 2 made of an InGaAlAs system is formed on an n-InP substrate 1 as an electro-absorption optical modulator using an MOCVD method. In this case, a light emission wavelength of the quantum well structure 2 at a temperature of 25° C. is about 1470 nm. For example, a desired light emission wavelength can be obtained by laminating a quantum well layer with a thickness of 6 nm and with a compositional ratio of In, Ga, and Al at 0.54:0.38:0.08, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.52:0.33:0.15. Further, an optical confinement structure sufficient for extinction can be formed as the quantum well structure by alternately laminating about 10 layers of the quantum wells and the barrier layers. Successively, etching is performed up to the surface of the n-InP substrate 1 while leaving the electro-absorption optical modulator of a desired length. The step is identical with the state shown in FIGS. 5A and 5B .
Then, a quantum well structure 3 made of an InGaAlAs system is formed as a semiconductor laser portion. The light emission wavelength of the quantum well structure 3 at a temperature of 25° C. is about 1540 nm. For example, a desired light emission wavelength can be obtained by forming a quantum well layer with a thickness of 4 nm and with a compositional ratio of In, Ga, and Al at 0.65:0.3:0.05, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.55:0.33:0.12. Further, an optical confinement structure suitable for laser oscillation can be formed by alternately laminating about 8 layers of the quantum wells and the barrier layers. Although not illustrated, a carrier confinement structure suitable for laser oscillation can be formed by sandwiching the quantum well structure 3 by InAlAs bulk growth layers with a thickness of about 100 nm and with a compositional ratio of In and Al at 0.52:0.48.
Etching is performed up to the surface of the n-InP substrate 1 while leaving the semiconductor laser portion of a desired length so as not to influence the electro-absorption optical modulator described above. The step is identical with the state shown in FIGS. 5C and 5D .
Then, an optical waveguide layer 4 made of an InGaAsP system is formed between the electro-absorption optical modulation portion and the semiconductor laser portion. As a detailed structure of the optical waveguide layer, for example, the following structure is desirable: an InGaAsP growth layer with a thickness of 100 nm and with the composition wavelength of 1150 nm is formed, an InGaAsP bulk growth layer with a thickness of 200 nm and with the composition wavelength of 1300 nm, and an InGaAsP bulk growth layer with a thickness of 100 nm and with the composition wavelength of 1150 nm are successively formed. An optical waveguide layer with a small optical loss can be formed by the structure described above. The step is identical with the state shown in FIG. 5D .
Then, a diffraction grating 5 is formed by etching on the quantum well structure 3 made of the InGaAlAs system as the semiconductor laser portion. As the diffraction grating layer, a semiconductor having a higher refractive index than that of InP is desired. For example, an InGaAsP grown layer with a thickness of 30 nm and with the composition wavelength of 1150 nm is suitable. In order to form the diffraction grating, pattern formation applied to a resist by a known technique of holographic exposure method or electron beam drawing method and a wet or dry etching step may be combined. As a specific resist pattern, stripes at a pitch of about 240 nm may be formed in the direction perpendicular to mesa. This can provide a stable longitudinal single mode oscillation suitable for optical communications. The step is identical with the state shown in FIG. 5E .
Then, a portion of the quantum well structure 2 made of the InGaAlAs system, which is formed as the electro-absorption optical modulator, is etched up to the n-InP substrate 1 to form a window structure 6 . The step is identical with the state shown in FIG. 5F .
Then, a p-InP layer 7 is formed on the entire surface by an MOCVD method. The step is identical with the state shown in FIG. 6A . Then, etching is performed up to the n-InP substrate 1 to form a ridged portion (high mesa structure) 13 . While the state is similar with that in FIG. 6B , the following points are different from FIG. 6B : since etching is performed up to the n-InP substrate 1 in Embodiment 2, the ridged portion 13 is stood upright on the substrate 1 , and the window structure 6 , the quantum well structure 2 , the optical waveguide layer 4 , and the quantum well structure 3 formed on the diffraction grating 5 are formed only for the base portion of the ridge portion 13 . In this case, a stable transverse single mode oscillation suitable for optical communications is obtained by defining the ridge with a width of about 2 μm.
Then, a semi-insulative InP layer is formed on both sides of the ridged portion 13 by an MOCVD method.
A silicon oxide film 8 is formed on the entire surface by a thermal CVD method. Then, the silicon oxide film 8 is removed only from the ridged portion 13 for the semiconductor light emission device and the electro-absorption optical modulation portion, the p-electrode 10 for the optical modulation portion, and the p-electrode 11 for the semiconductor laser portion. While the silicon oxide film is used in Embodiment 2, a silicon nitride film or the like may also be used instead.
Then, a p-electrode 10 for the optical modulation portion and a p-electrode 11 for the semiconductor laser portion are formed. As the electrode material, known Ti and Au may be formed successively. Then, an n-electrode 12 is formed at the rear face of then-InP substrate 1 . As the electrode material, known AuGe, Ti, and Au may be formed successively in the same manner.
After forming the electrode, the device is cut out by cleavage and a reflection film with reflectivity of 90% is formed at the rear end surface and a low reflection film with a reflectivity of 1% or less are formed at the front edge surface by a sputtering method.
According to the method described above, a buried hetero type semiconductor optical integrated device in which the EA modulator portion and the DFB laser portion are integrated on one identical substrate can be formed. The order of crystal growth for the EA modulation portion, the waveguide portion, and the DFB laser portion is not limited to that described above. For example, also in the case of forming the DFB laser portion at first, the obtained device structure does not change. With respect to the material for the electro-absorption optical modulator, it may be a quantum well structure in which the well layer is made of any one of InGaAlAs, InGaAsP, and InGaAs, and the barrier layer is made of either one of InGaAlAs or InAlAs. As the material for the semiconductor laser portion, an InGaAsP system may be used instead of the InGaAlAs system. As the material for the optical waveguide, an InGaAlAs system may also be used instead of the InGaAsP system. Further, the method of crystal growth is not necessarily restricted to the MOCVD method and an MBE method may be used for formation. Further, the EA modulation portion, the waveguide portion and, the DFB laser portion may be formed in one crystal growth step by using a selective area growth method. Further, a bent waveguide structure may also be used instead of the window structure.
According to the procedures described above, a method of manufacturing a device in the case where the DFB laser portion is replaced with a DBR laser, a SOA, or the like may also be inferred easily.
The operation method of the semiconductor optical integrated circuit device according to Embodiment 2 is the same as that in Embodiment 1.
Embodiment 3
RWG-EA/Variable Wavelength LD
FIG. 8A is a perspective view showing the constitution according to another embodiment of a semiconductor optical integrated device formed as a variable wavelength LD applied to the present invention. FIG. 8B is a perspective view illustrating a cross section cut along a central line. Figures for the processes shown in FIGS. 5 and 6 in Embodiment 1 are not illustrated. However, the drawing is only for the explanation of this embodiment and the size and scale of the drawing showing this embodiment are not necessarily identical.
A quantum well structure 2 made of an InGaAlAs system is formed on an n-InP substrate 1 as an electro-absorption optical modulator using an MOCVD method. In this case, a light emission wavelength of the quantum well structure at a temperature of 25° C. is about 1470 nm. For example, a desired light emission wavelength can be obtained by forming a quantum well layer with a thickness of 6 nm and with a compositional ratio of In, Ga, and Al at 0.54:0.38:0.08, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.52:0.33:0.15. Further, an optical confinement structure sufficient for extinction can be formed as the quantum well structure 2 by alternative laminating about 10 layers of the quantum wells and the barrier layers. Successively, etching is performed up to the surface of the n-InP substrate 1 while leaving the electro-absorption optical modulator of a desired length. The step is the same as the state shown in FIGS. 5A and 5B .
Then, a quantum well structure 3 made of an InGaAlAs system is formed as a semiconductor laser portion. The light emission wavelength of the quantum well structure 3 at a temperature of 25° C. is about 1540 nm. For example, a desired light emission wavelength can be obtained by forming a quantum well with a thickness of 4 nm and with a compositional ratio of In, Ga, and Al at 0.65:0.3:0.05, and a barrier layer with a thickness of 10 nm and with a compositional ratio of In, Ga, and Al at 0.55:0.33:0.12. Further, an optical confinement structure suitable for laser oscillation can be formed by alternately laminating about 7 layers of the quantum wells and the barrier layers. Although not illustrated, a carrier confinement structure suitable for laser oscillation can be formed by sandwiching the quantum well structure 3 between InAlAs bulk growth layers with a thickness of about 100 nm and with a compositional ratio of In and Al at 0.52:0.48.
Successively, etching is performed up to the surface of the n-InP substrate 1 without any influence on the electro-absorption optical modulator described above while leaving the electro-absorption optical modulation portion, an active region 15 and a phase control region 16 . The active region 15 and the phase control region 16 , each with a desired length, are formed at the quantum well structure 3 . The step is the same as the state shown in FIGS. 5C and 5D . In the variable wavelength LD, however, the optical waveguide layer 4 is formed on the side of the phase control region 16 . The phase control region 16 with the desired length is formed at the quantum well structure 3 . The side of the phase control region 16 is on the opposite side to the electro-absorption optical modulation portion. Thus, etching is performed up to the surface of the n-InP substrate 1 for the predetermined length on the opposite side to the electro-absorption optical modulation portion.
Then, an optical waveguide layer 4 made of an InGaAsP system is formed between the electro-absorption optical modulation portion and the active region 14 with the desired length at the quantum well structure 3 and is formed in the region adjacent with the phase control region 16 with the desired length at the quantum well structure 3 . As a detailed structure of the optical waveguide layer 4 , it is desired that a structure is formed, for example, by laminating an InGaAsP bulk growth layer with a thickness of 100 nm and with a composition wavelength of 1150 nm, an InGaAsP growth layer with a thickness of 200 nm and with a composition wavelength of 1300 nm, and further laminating an InGaAsP bulk growth layer with a thickness of 100 nm and with a composition wavelength of 1150 nm is desired. With the structure described above, an optical waveguide layer with a small optical loss can be formed.
Then, a diffraction grating 5 is formed by etching in a desired region of the optical waveguide layer 4 made of the InGaAsP system in the region adjacent with the phase control region 15 to form a distributed reflection type region 17 . In order to form the diffraction grating, pattern formation to a resist using either a holographic exposure method or an electron beam drawing method, both of which are known techniques, and either of a wet or dry etching step may be combined.
A portion of the quantum well structure 2 is made of the InGaAlAs system and is formed as the electro-absorption optical modulator. The portion of the quantum well structure 2 on the side of light emission edge is etched up to the n-InP substrate 1 in order to form a window structure 6 . The step is the same as the state shown in FIG. 5( f ).
Then, a p-InP layer 7 is formed by an MOCVD method. The step is the same as the state shown in FIG. 6( a ). A ridged waveguide structure 13 is formed by etching the p-InP layer 7 up to the surfaces of the quantum well structure 2 , the quantum well structure 3 , and the optical waveguide layer 4 except for the portion for forming the ridged waveguide. The quantum well structure 2 is made of the In, Ga, Al, and As systems and is formed as the electro-absorption optical modulator. The quantum well structure 3 is made of the InGaAlAs system and is formed as the semiconductor laser portion. The step is the same as the state shown in FIG. 6( b ). A stable transverse single mode oscillation suitable for optical communications can be obtained by defining the ridge with a width of about 2 μm.
A silicon oxide film 8 is formed over the entire surface by a thermal CVD method. The step is the same as the state shown in FIG. 6( c ). The silicon oxide film 8 is removed from the ridged portion 13 at the positions corresponding to electrodes 10 , 18 , 19 , and 20 . This will be described later. While the silicon oxide film is used in Embodiment 3, a silicon nitride film or the like may also be used instead.
The wafer is planarized at the height of the top surface of the ridge 13 on which the silicon oxide film 8 is removed by a polyimide resin 9 . Then, a p-electrode 10 for the optical modulation portion, a p-electrode 17 for the active region, and a p-electrode 18 for the phase control region, and a p-electrode 19 for distributed reflection type region are formed. For the electrode materials, known Ti and Au may be successively formed. Then, an n-electrode 12 is formed to the rear face of the n-InP substrate 1 . For the electrode material, known AuGe, Ti, and Au may be successively formed in the same manner.
After forming the electrode, the device is cut out by cleavage. A reflection film with reflectivity of 90% is formed at the rear end surface and a reflection film with a reflectivity of 1% or less is formed to the front end surface by a sputtering method.
According to the method described above, a ridged waveguide type semiconductor optical integrated device in which the EA modulator portion and the variable wavelength laser portion are integrated on one identical substrate can be formed. The order of crystal growth for the EA modulation portion, the waveguide portion, and the tunable wavelength laser portion is not limited to that described above. With respect to the material for the electro-absorption optical modulator, it may be a quantum well structure in which the well layer is made of any one of InGaAlAs, InGaAsP, and InGaAs, and the barrier layer is made of either one of InGaAlAs or InAlAs. For the material for the variable wavelength laser portion, an InGaAsP system may be used instead of the InGaAlAs system. For the material for the optical waveguide, an InGaAlAs system may also be used instead of the InGaAsP system. The method of crystal growth is not necessarily limited to the MOCVD method. For example, an MBE method may be used. Further, the EA modulation portion, the waveguide portion, and the DFB laser portion may be formed in one crystal growth step by using a selective area growth method. Further, a bent waveguide structure may also be used instead of the window structure. Further, the method of manufacturing the buried hetero device may be inferred easily from Embodiments 1 and 2. Further, planarization by the polyimide is not necessarily required.
Then, the operation method of the semiconductor optical integrated device of Embodiment 3 will be described. Laser oscillation is obtained by applying a forward bias to the p-electrode 18 for the active region. In this case, since the light is periodically fed back by the distributed reflection region 17 , the oscillation spectrum exhibits a single mode. By supplying current to the p-electrode 20 for the distributed reflection region, Bragg's reflection condition can be changed to change the laser oscillation wavelength. Further, by supplying current to the p-electrode 19 for the phase control region, continuous variable wavelength can be attained without a mode hop.
Also, the light modulation method in Embodiment 3 may be inferred easily from Embodiment 1.
Embodiment 4
Module Using EA/DFB
In an embodiment of a transmitter/receiver module using the semiconductor optical integrated device described in Embodiment 1 and Embodiment 2, the outline of the structure is explained with reference to FIG. 9 and the outline of the control system is explained with reference to FIG. 10 . However, the drawings are only for the explanation of this embodiment, and the size and scale of the drawings showing this embodiment do not always identical.
Numeral 21 represents a small-sized optical transmitter module in which a semiconductor optical integrated device 22 formed by integrating a laser portion 31 and an optical modulator 32 , both of which support the uncooled operation of the invention, is mounted on an internal substrate 21 ′. At the top end of the module 21 , a lens 25 is maintained by a lens support 25 ′. The semiconductor optical integrated device 22 and the lens 25 are arranged such that the optical axis of light generated from the laser portion 31 is matched. A thermistor 23 is disposed near the semiconductor optical integrated device 22 on the internal substrate 21 ′ to output a signal for temperature in the module. Behind the semiconductor optical integrated device 22 , a monitor photodetector 24 is disposed to detect the optical output due to the backward leak of the laser portion 31 . The output from the monitor photodetector 24 is utilized as the operation temperature signal of the laser portion 31 . A control device 29 is disposed adjacent with the small-sized optical transmission module 21 . The control device 29 is provided with an optical modulator control circuit 33 and an optical laser portion control circuit 34 . Lead lines 27 are disposed between the small-sized optical transmission module 21 and the control device 29 to perform a necessary signal transfer between them. Wires 28 are for connection between the lead lines 27 and each of the devices. A high frequency line 26 gives a signal from the optical modulator control circuit 33 to the optical modulator 32 . An electric signal in accordance with the intensity of the light incident to the monitor photodetector 24 is sent through the wires 28 and lead wires 27 to the optical laser control circuit 34 on the control device 29 . A feedback control is applied to the value of current flowing to the laser portion 31 on the semiconductor optical integrated device 22 so as to obtain a desired optical output.
As described above, the temperature in the small-sized optical transmitter module 21 is monitored by the thermistor 23 to control the optical modulator 32 . The operation temperature of the laser portion 31 is monitored by the monitor photodetector 24 to control the laser portion 31 . Thus, the semiconductor light emitting device which is constituted so as to attain the characteristic shown in FIG. 3 can be used as an optical transmitter which does not require temperature control. While the control circuit and the device constituting the module are connected through the wires and the leads, they may be monolithically integrated on one chip. With this module, a high speed optical signal can be easily produced. This is suitable for reduction in size, reduction in power consumption, and long distance transmission. The variable wavelength semiconductor optical integrated circuit is not explained in FIGS. 9 and 10 .
Embodiment 5
Optical Communication System
FIG. 11 is a schematic view showing a terminal of an optical communication system constituted by an optical transmitter/receiver package in which an optical transmission module of the present invention shown in FIG. 9 and FIG. 10 , and an optical receiving module separately assembled are mounted. Numeral 37 denotes the optical transmitter/receiver package. Numeral 35 denotes an optical transmission module. Numeral 38 denotes an optical transmission module driver circuit. Numeral 36 denotes an optical receiving module. Numeral 39 denotes an optical receiving module driver circuit. Numerals 40 and 41 denote optical fibers which are disposed corresponding to the optical transmission module 35 and the optical receiving module 36 , respectively. | In a conventional EA/DFB laser, since the temperature dependence of the operation wavelength of the EA portion is substantially different from that of the DFB portion, the temperature range over which a stable operation is possible is small. In the case of using the EA/DFB laser as a light emission device, an uncooled operation is not possible. An EA/DFB laser which does not require a temperature control mechanism is proposed.
A quantum well structure in which a well layer made of any one of InGaAlAs, InGaAsP, and InGaAs, and a barrier layer made of either one of InGaAlAs or InAlAs is used for an optical absorption layer of an EA modulator. By properly determining detuning at a temperature of 25° C. and a composition wavelength of the barrier layer in the quantum well structure used for the optical absorption layer, it can be realized to suppress the insertion loss, maintain the extinction ratio, and reduce chirping simultaneously over a wide temperature range from −5° C. to 80° C. | 6 |
BACKGROUND OF THE INVENTION
This invention relates to a carton folding mechanism for a machine for packaging articles in, for example, a sleeve type wraparound carton. Typically the carton is formed from a paperboard blank in which a side wall panel and base panel are hinged together along a fold line. Article apertures, for example, bottle heel retaining apertures incorporating hinged retaining flaps are disposed astride the fold line between the carton panels. The machine in which the mechanism of the present invention may be incorporated includes a conveyor for advancing a blank and the articles to be packaged along a predetermined feed path. The mechanism folds such retaining flaps into their required positions inwardly of the carton. The present invention is concerned with the inward folding of pairs of such retaining flaps associated with each article retention apertures. The flaps of each pair of flaps are engaged and folded inwardly while the adjacent portions of the blank are held against any substantial sidewise movement by suitable guide means.
It is known from EP-0 200 445 to provide article retaining features such as bottle heel retention apertures in the base and side walls of a wraparound carton which receive a heel portion of an article such as a bottle packaged in the carton. Such heel retaining features normally are struck from the side and base wall panels of a wraparound carton and comprise flaps which are hingably attached to the carton panel. In the flat blank the flaps close the apertures which are to provide the bottle heel retention apertures of the carton. When the blank is applied to a group of articles, it is known to open the flaps using a simple finger mechanism to later enable the heel of the article to be received in the aperture created.
A mechanism for achieving this function is disclosed in EP-0 200 445 and comprises a mechanism for engaging and folding a pair of bottle heel retention flaps so that the flaps are folded inwardly of the carton. The folding mechanism includes a pivotal folder comprising a pair of pivotal fingers which are cam actuated so as to execute a folding movement whereby the fingers progressively enter a retention aperture in the blank to fold the flaps and to execute a retracting movement. These folding and retracting movements occur during linear feed movement of the carton blank and the pivotal folder together. The pivotal folders operate sequentially upon a blank to fold open a row of such heel retention flaps and, in a folding section of the machine, move together with the blank through the machine. In order to actuate the pivotal fingers each pivotal folder engages a fixed cam track formed in a cam block and is conveyed through a working path and a return path of a chain and sprocket assembly.
SUMMARY OF THE INVENTION
The invention provides a device for use in a machine for packaging articles in a wraparound carrier of the type formed from a blank having a pair of walls adjoined together along a fold line and having a pair of article retaining and blank reinforcing flaps disposed astride said fold line said device comprising folding means for engaging and folding said pair of flaps and to fold such flaps inwardly of the carrier, said folding means comprising a folder adapted to execute a folding movement thereby progressively to enter an aperture in the blank to fold the flaps and to retract therefrom during feed movement of the blank, said folder including a blank engaging portion and means for cooperation with actuating means to pivot the blank engaging portion thereby to execute said folding movement and said retracting movement wherein said folder is radially movable with respect to an axis of the device and said blank engaging portion comprises a pair of divergently pivotal fingers adapted to pivot upon radial movement of the folder with respect to said axis.
According to a feature of the invention, said cooperating means may comprise a cam follower which rides in an endless cam track contoured so as to cause said folding movement and said retracting movement.
According to another feature of the invention, said folding means may comprise a rotatable plate assembly incorporating said folder and said endless cam track.
In constructions where a plate assemble is provided the plate assembly may comprise, in axial series, a cam plate, an intermediate plate incorporating said folders and a top plate and wherein the intermediate and top plates are rotatable relative to the cam plate. Preferably, the plates are discs.
According to yet another feature of the invention, said folder may comprise a body which is mounted for radial movement in said intermediate plate which body carries said cam follower. The body may terminate in a head comprising a pair of pivotal fingers which provide the blank engaging portion of said folder. Preferably, the pivotal fingers are caused to pivot substantially simultaneously and cooperate with parts of said intermediate plate to effect their pivotal movement.
According to a still further feature of the invention said body may be slidably mounted in a radial track provided in the intermediate disc.
According to another feature of the invention said plate assembly may comprise a plurality of folders arranged in discrete groups whereby a separate one of each group of folders is provided for each successive carton to be engaged.
BRIEF DESCRIPTION OF THE DRAWINGS
An embodiment of the invention will now be described, by way of example only, with reference to the accompanying drawings, in which:
FIGS. 1 to 10 show different stages of the following operation of a mechanism according to the invention;
FIG. 11 shows a schematic perspective view of the mechanism according to the invention shown partly broken away;
FIG. 12 is a perspective view of part of the mechanism shown in FIG. 11;
FIG. 13 is a plan view of a pivotal finger which forms part of a folder device according to the invention; and
FIG. 14 is a sectional side view of the finger shown in FIG. 13.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to the drawings, FIGS. 1 to 10 are a schematic representation of the operation of a carton flap opening mechanism 10 according to the invention. The mechanism comprises a number of sets of rotatably mounted folders to cooperate sequentially with a carton blank adapted to provide two heel retention apertures at each side of the carton. FIGS. 1-10 illustrate the sequential steps during rotation of a rotatable plate assembly 36, 38 on which a pair of such folders 12 are carried to effect the opening of heel retention apertures A by, in each case, displacing a pair of flaps f 1 , f 2 of a carton blank C. In this case the carton blank is of the wraparound type. The heel portions of a pair of bottles B 1 , B 2 are then received in respective ones of the retaining apertures A.
FIG. 11 is a schematic perspective view of the rotatable disc plate mechanism 10 which comprises an upper disc 38, an intermediate disc 36 and a lower fixed cam plate 34. The discs can be driven, for example, by a shaft fixed to each of the discs and rotatably journalled through the centre of the fixed cam plate. The shaft may of course be connected to be driven through some suitable form of mechanical linkage to a motor in order to effect the correct rotational speed of the wheel assembly in synchronisation with the movement of the carton blank C in the packaging process. The opening mechanism 10 in this example, comprises three series of four closely and equally spaced folders. The number and spacing of each of the folders 12 is determined by the type of carton being used to package articles. In this specific example, the cartons are configured to package a 4×2 arrangement so that a row of four articles will be disposed along each side wall of the carton. Hence, since there are three groups of four pivotal folders, one revolution of the wheel assembly will effect the opening of heel retention flaps in three successive carton blanks. The carton C comprises a side wall having apertures A for receiving heel portions of articles B and flaps "f" struck from the carton side wall which are required to be opened out of the flat plane of the side wall, inwardly of the carton.
A pair of blank folding mechanisms 10 is adapted to be installed adjacent the infeed end of a packaging machine. Two such mechanisms are installed in side-by-side relationship so that a blank and article feed path is provided between the mechanisms. The description hereinafter refers to only one mechanism of the pair the other mechanism being similar in all aspects. The carton blank is formed with a linear series of article heel retaining apertures A which are struck along the fold line which foldably connects a side wall panel with a bottom panel of the blank. Such heel retaining apertures are provided to receive e.g. heel portions of bottles to assist retention of the bottles in the completed carton. The heel retaining apertures are each defined in part, by foldable reinforcing flaps f which are foldable, to open the aperture, into overlapping relationship with adjacent portions of the side wall and base panel of the blank.
An individual folder 12 from one of the three groups is shown in FIG. 11 wherein first and second fingers 14 and 16, respectively, are shown in their fully opened position in which they protrude from recess 40 in disc 36. Each pivotal folder comprises an elongate rod 26 which is received in a radial track 28 formed in intermediate disc 36 for reciprocal movement therein. The radially outer end of rod 26 carries a head plate 24 formed with an ovate transverse opening 22. The pivotal fingers 14 and 16 have upper locating pins 18 and 20 respectively which are slidably received in opening 22 and each have a lower locating pin 52 which are each received in a recess 50 formed in a protruding portion 37 of disc 36. The latter components are shown in FIGS. 12 to 14. It can be seen from the plan view of FIG. 13 that pin 20 is displaced from the centre of pin 52 in order to effect the opening movement of fingers 14 and 16 during radial movement of rod 26. Preferably the angle A subtended by the axis of pin 20 at the axis of pin 52 relative to a line R' parallel to radial edge R of finger 16, which edge forms the edge which abuts finger 14, is in the order of 45°.
A cam follower, in this case a roller assembly 30, depends from the lower face of rod 26 intermediate its ends and rolls in a cam track 32 formed in cam plate 34. The pivotal fingers 14 and 16 are caused to move through the action of the reciprocating rod 26 which moves radially inwardly and outwardly along the radial track 28 in response to radial movement of the cam follower 30 in cam track 32. The cam track 32 is shown schematically in each of the FIGS. 1 to 10 and thus the location of fingers 14 and 16 with respect to their position in relation to cam track 32 can be followed in each of the same figures. As is apparent, the pivotal fingers are opened to their maximum extent (as shown in FIG. 11) when reciprocating rod 26 is at its radially outermost limit and thus when cam follower 30 reaches the most eccentric part of cam track 32.
FIG. 11 is, of course, only schematic, and it is apparent that each protruding portion 13 of upper disc 38 is provided in its lower surface with a radial groove (not shown) for receiving head plate 24 thereby to enable radial movement of head plate 24.
Referring again to FIGS. 1 to 10 it can be seen that as the disc assembly 36, 38 is caused to rotate clockwise, a first folder 12 engages a carton blank and penetrates an aperture A thus separating the flaps f 1 , f 2 from co-planar alignment with the side panel of the carton. In FIG. 1, folder 12 has rotated into abutment with the side of carton blank C, whereas in FIG. 2, further rotation has caused initial penetration of folder 12 into the heel retaining aperture A.
FIG. 3 illustrates folder 12 at a position where it has almost entirely penetrated the aperture A causing the flaps f 1 , f 2 to fold inwardly away from one another significantly, but not beyond a 90° position relative to the carton side panel. This is the situation also for the next sequence of events up to and including the position shown in FIG. 5. It will be appreciated that up to this position the pivotal fingers of the folder 12 remain closed even though they have penetrated the blank.
In FIG. 6 the pivotal fingers 14 and 16 begin to pivot apart from one another and thus open folding flaps f 1 , f 2 still further.
In FIG. 7 the flaps f 1 , f 2 have been folded beyond the 90° position relative to the associated carton side wall and begin to be folded towards adjacent parts of the carton side wall. The second folder 12 1 is at that time beginning to penetrate the next adjacent aperture A 1 having flaps f 3 , f 4 .
In FIG. 8 cam follower 30 has reached the radially outermost part of cam track 32 and thus reciprocating rod 26 causes head plate 24 to reach its radially outermost position. Hence, this causes maximum opening of the pivotal fingers 14 and 16 due to the action of plate 24 on locating pins 18 and 20 received in groove 22.
FIG. 9 shows that cam follower 30 has passed the radially outermost extent of cam track 32 and that rod 26 is caused to retract thereby causing the pivotal fingers 14 and 16 to begin to close back together.
in FIG. 10 the pivotal fingers 14 and 16 are brought even closer together and thereby enable the fingers to be retracted from the aperture A.
Thus, when the fingers are pivoted into their extreme outward position, the fingers move apart to engage and fold outwardly the tabs of the heel retaining aperture and when the fingers are pivoted into their fully retracted position, the fingers are closed together.
During this operation it is apparent from the schematic drawings 1 to 10 that the pivotal fingers operate adjacent the bases of the bottles, B 1 , B 2 . The bottle heels are then engaged in their respective heel apertures as the carton side panels move inwardly. This occurs by bringing the carton base panels into overlapping relationship which has the general effect of `tightening` the carton blank about the group of bottles. In this specific example, all four adjacent apertures will have been opened before the wraparound carton is closed about the group of bottles.
It is apparent from the drawings that the pivotal fingers 13,14 of the folders have a curved outer profile in order better to effect penetration of aperture A and to enable a progressive folding effect in the expansion of the flaps f 1 , f 2 . It will be appreciated that an opening mechanism 10 according to the invention can be readily modified so as to operate in conjunction with cartons of a different configuration to those described here. Thus change-over from one carton form to another different form simply requires the removal of the current disc assembly and the substitution of another appropriate disc assembly whose diameter, pivotal finger grouping and number and rotational speed of the assembly are matched to the type of carton to be run on the machine. This is in contrast to the considerably more laborious change-over requirements of the known mechanism in which the number and spacing of the pivotal fingers often would need to be individually adjusted on the endless chain assembly. | A flap-folding device for use in a packaging machine comprises a rotational disc, drive means for rotating the disc in synchronization with movement of a blank and articles to be packaged in the blank, a pair of blank-engaging fingers pivotally mounted on the disc to fold flaps on the blank, and actuating means for pivotally moving the fingers. The actuating means comprises a radial member mounted on the disc for reciprocating movement along the radius of the disc, cooperating means for moving the radial member along the radius in response to rotation of the disc, and means for converting reciprocating movement of the radial member into pivotal movement of the fingers. | 1 |
REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to United Kingdom Patent Application GB 0603242.9 filed on Feb. 17, 2006.
BACKGROUND OF THE INVENTION
[0002] The present invention relates generally to latch assemblies, and in particular to latch assemblies for use with car doors and car boots (trunks).
[0003] Latch assemblies are known to releasably secure car doors in a closed position. Operation of an inside door handle or an outside door handle will release the latch, allowing the door to open. Subsequent closure of the door will automatically relatch the latch.
[0004] To ensure that rain does not enter the vehicle, weather seals are provided around a peripheral edge of the doors which close against an aperture in a vehicle body in which the door sits. In addition to providing protection from the rain, the weather seals also reduce the wind noise. The ongoing requirement for improved vehicle occupant comfort requires minimization of wind noise, which in turn requires the weather seals to be clamped tighter by the door. The door clamps the seals by virtue of the door latch. Accordingly, there is a tendency for a seal load exerted on the door latch to be increased to meet the required increased occupancy comfort levels. Because the seal force on the latch is increased, the forces required to release the latch are correspondingly increased.
[0005] U.S. Pat. No. 3,386,761 shows a vehicle door mounted latch having a rotatable claw which releasably retains a vehicle body mounted striker to hold a door in a closed position. The rotatable claw is held in the closed position by a first pawl, and the first pawl is held in the closed position by a second pawl. The second pawl can be moved to a release position by an electric actuator, which in turn frees the first pawl, which allows the rotatable claw to rotate to an open position. The system is arranged such that once the second pawl has disengaged the first pawl, the first pawl is driven to a release position by the seal load acting on the rotatable claw.
[0006] US2004/0227358 shows a rotatable claw held in a closed position by a rotatable lever and a link. The rotatable lever can in turn be held in position by a pawl. Disengaging the pawl from the rotatable lever allows the rotatable lever, the link and the pawl to move to an open position. One end of the link remains in permanent engagement with the rotatable claw. The system is arranged such that once the pawl has disengaged from the rotatable lever, the rotatable lever and the link are driven to the open position by the seal load acting on the rotatable claw.
[0007] EP0978609 shows a rotatable claw that can be held in a closed position by a pawl. The pawl is mounted on a cam. During an initial part of opening of a latch, the cam rotates relative to the pawl, thereby initially slightly increasing and then significantly reducing a seal load. During a final part of opening of the latch, the cam and the pawl rotate in unison, thereby disengaging a pawl tooth from a claw tooth. However, the arrangement is such that the cam must be driven by a motor to release the latch. In particular, in the closed position, the particular configuration of a cam axis, a pawl pivot axis and a pawl tooth is such that latch will remain shut. Thus, in the closed position, the pawl pivot axis (28 of EP0978609) lies just to one side of a line (31 of EP0978609) drawn between the cam axis and a point where the pawl tooth contacts the rotatable claw. Significantly, the pawl pivot axis must move towards this line for the latch to be opened. In other words, the pawl is at an over-center position such that the cam is driven in a closing direction when the latch has been closed.
[0008] DE10214691 and U.S. Pat. No. 5,188,406 are similarly in an overcenter position when in the closed position.
[0009] Thus, EP0978609, DE10214691 and U.S. Pat. No. 5,188,406 all show latches in which the component in direct contact with the claw (the pawl) is in a stable position. U.S. Pat. No. 3,386,761 and US2004/0227358 both show latches wherein the component in direct contact with the claw is in an unstable position and therefore requires a further component (the second pawl in U.S. Pat. No. 3,386,761 and the pawl in US2004/0227358) to hold the component that directly engages the claw in the unstable position.
SUMMARY OF THE INVENTION
[0010] An object of the present invention is to provide a compact latch arrangement. Another object of the present invention is to provide a reduced force release latch that is reliable in operation.
[0011] Thus, the present invention provides a latch assembly including a chassis and a rotatable claw-type latch bolt moveably mounted on the chassis. The latch bolt has a closed position for retaining a striker and an open position for releasing the striker. The latch bolt is provided with a latch abutment remote from a center of rotation. The latch assembly further includes a pawl having an engaged position for holding the latch bolt in the closed position and a disengaged position that allows the latch bolt to move to the open position. The latch assembly includes an eccentric arrangement defining a first axis and a pawl axis remote from the first axis. The pawl is rotatable about the pawl axis. The latch assembly also includes a reset lever rotatably fixed to the eccentric arrangement for mutual rotation with the eccentric arrangement about the first axis. A biasing lever is configured to transmit a biasing force to the reset lever at a position remote from the first axis and to the latch bolt via the latch abutment. The latch assembly includes a biasing device arranged to apply the biasing force to the biasing lever. The latch assembly is configured such that when the pawl retains the latch bolt in the closed position, the biasing lever applies a force to the reset lever to promote disengagement of the pawl, and such that when the pawl is disengaged, the biasing lever promotes the rotation of the latch bolt into the open position.
[0012] According to another aspect of the present invention, a method of operating the latch assembly from a closed position to an open position includes the steps of releasing the eccentric arrangement for rotation about the first axis, rotating the reset lever with the biasing lever to disengage the pawl, and rotating the latch bolt with the biasing lever into the open position once the pawl has retracted to a predetermined extent.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] The invention will now be described, by way of example only, with reference to the accompanying drawings in which:
[0014] FIG. 1 is a view of a backplate side of a latch of certain components of a latch arrangement according to the present invention in a closed position, and with the backplate omitted;
[0015] FIG. 1A is a view of the backplate side of the latch of certain components of the latch arrangement in the closed position, with the backplate omitted;
[0016] FIG. 1B is a view of the backplate side of the latch with further components in place in the closed position;
[0017] FIG. 1C is a view of the backplate side of the latch with further components in place in an opening position, respectively;
[0018] FIG. 2 is a view of the backplate side of the latch of certain components of the latch arrangement of FIG. 1 in the closed position with further components in place, and the backplate omitted;
[0019] FIG. 3 shows certain components of FIG. 2 in a released but not fully open condition while the latch is being opened; and
[0020] FIG. 4 shows the same components as FIGS. 2 and 3 in a fully open position.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0021] With reference to the Figures, a latch assembly 10 includes a latch chassis 12 , a latch bolt in the form of a rotatable claw 14 , a pawl 16 , an eccentric arrangement in the form of a crank shaft assembly 18 and a release actuator assembly 20 . The latch assembly 10 is mounted on a door 8 (only shown in FIG. 1 ).
[0022] The major components of the latch chassis 12 are a retention plate 22 and a backplate 24 ( FIG. 1C ). The retention plate 22 is generally planar and includes a mouth 26 for receiving a striker (not shown). The retention plate 22 includes three threaded holes 27 whose edges are bent over to project out of the paper as shown in FIG. 1 , which in use secure the latch assembly 10 to the door 8 . A claw pivot pin 28 and stop pins 29 and 30 protect from the retention plate 22 . The stop pin 29 includes a cylindrical outer surface 29 A, the purpose of which will be described below.
[0023] The backplate 24 ( FIG. 1C ) includes holes 31 A and 31 B for receiving ends of the claw pivot pin 28 and the stop pin 29 , respectively. During assembly, the ends of the claw pivot pin 28 and the stop pin 29 are peened over to secure the backplate 24 relative to the retention plate 22 .
[0024] The claw 14 is pivotally mounted on the claw pivot pin 28 and includes a mouth 32 for receiving the striker, a first safety abutment 33 and a closed abutment 34 . The claw 14 is generally planar and includes a biasing pin 37 which projects out of the general plane of the claw 14 .
[0025] The pawl 16 includes a pawl tooth 40 , a first arm 41 having an abutment surface 42 , and a second arm 43 . The pawl 16 also has a pawl pivot hole 46 of an internal diameter D. The pawl 16 is biased in a counter-clockwise direction about a crank pin axis Y (see below) by a spring 47 engaging the second arm 43 when viewing FIG. 1 .
[0026] The major components of the crank shaft assembly 18 are a crank shaft 50 , a reset lever 51 ( FIGS. 2-4 ) and a release lever 52 ( FIGS. 1B and 1C ).
[0027] The crank shaft 50 includes a crank pin 54 in the form of disc having a crank pin axis Y. A square shaft 55 projects from one side of the crank pin 54 , and a cylindrical pin 56 (shown in broken lines in FIG. 1 ) projects from the other side of the crank pin 54 . In other embodiments, alternative forms of the crank shaft 50 may be provided (e.g., other non-circular profiles) to cause components to be rotationally fixed thereto. The square shaft 55 and the cylindrical pin 56 together define a crank shaft axis A. The cylindrical pin 56 is rotatably mounted in a hole (not shown) of the retention plate 22 . The retention plate 22 thereby provides a bearing for the cylindrical pin 56 . An end of the square shaft 55 is provided with a threaded hole 57 .
[0028] The diameter of the crank pin 54 is a running fit in the pawl pivot hole 46 , i.e., the diameter of the crank pin 54 is slightly less than the internal diameter D. The crank pin axis Y therefore defines a pawl axis about which the pawl 16 can rotate (see below). The thickness of the crank pin 54 is substantially the same as the thickness of the pawl 16 .
[0029] A reset lever 51 is fitted to the square shaft 55 directly above the crank pin 54 and includes a first arm 60 , a second arm 63 and a boss 61 secured intermediate the first arm 60 and the second arm 63 . The boss 61 has a cylindrical outer surface 62 and a central hole of square cross section. Accordingly, when the reset lever 51 is assembled onto the square shaft 55 , as shown in FIG. 2 , the first arm 60 becomes rotationally fixed with the crank shaft 50 . The cylindrical outer surface 62 of the boss 61 is mounted in a hole in the backplate 24 , which thereby provides a bearing surface for the cylindrical outer surface 62 . The cylindrical outer surface 62 and the outer surface of the cylindrical pin 56 are concentric and together define the crank shaft axis A.
[0030] A biasing lever 80 is pivotably mounted to the second arm 63 proximate a first end 81 of the biasing lever 80 and extends above the pawl 16 and the claw 14 to contact the biasing pin 37 of the claw 14 proximate a second end 82 of the biasing lever 80 . The biasing lever 80 is further provided with a spring abutment 83 intermediate the first end 81 and the second end 82 and a biasing lever nose 84 offset from a plane of the biasing lever 80 to be capable of contacting the reset lever 51 .
[0031] A biasing device in the form of a torsion spring 85 is secured to the retention plate 22 by the coil portion 86 that encircles one of the threaded holes 27 and a first leg 87 that is retained by a lug 88 of the retention plate 22 . A second spring leg 89 contacts the spring abutment 83 to apply a force FB to the biasing lever 80 that acts towards the right as illustrated in FIG. 2 . A component of this force is transmitted both to the pivotable connection with the reset lever 51 as a force FR and by the contact between the biasing lever 80 and the biasing pin 37 as a force FC, when the claw 14 is in a closed position.
[0032] The 60 includes an edge 60 A (also known as a reset abutment) which interacts with the biasing lever nose 84 , as will be described further below. The release lever 52 is generally elongate and includes a square hole 64 at one end to receive an end of the square shaft 55 and a release abutment 65 at the other end.
[0033] A bolt and washer (not shown) is screwed into the threaded hole 57 of the square shaft 55 to secure the crank shaft 50 , the reset lever 51 and the release lever 52 together. Accordingly, the crank shaft 50 , the reset lever 51 and the release lever 52 are all rotationally fixed relative to each other.
[0034] When assembled, the crank pin 54 and the reset lever 51 are positioned between the retention plate 22 and the backplate 24 with a cylindrical outer surface 62 of the boss 61 being rotationally mounted in a hole (not shown) of the backplate 24 . The release lever 52 lies on an opposite side of backplate 24 to the reset lever 51 and the crank pin 54 (best shown in FIG. 1C ).
[0035] The major components of the release actuator assembly 20 are a bracket 70 , an electromagnet 71 and a release plate 72 . The bracket 70 is bent from the backplate 24 and is used to mount the electromagnet 71 . The bracket 70 is also used to pivotally mount the release plate 72 , which is made from a magnetic material, such as steel. The release plate 72 is planar and generally rectangular in plan view and it can be seen from FIG. 1B that it projects equally either side of where it pivots on the bracket 70 . Thus, the release plate 72 is balanced.
[0036] The release plate 72 is biased in a counter-clockwise direction when viewing FIG. 1B by the spring 73 (shown schematically). The release plate 72 includes an abutment 74 at one end. Other suitable forms of release actuator known in the art may be employed.
[0037] Operation of the latch assembly 10 is as follows. Consideration of FIGS. 1, 1A , 1 B and 2 show the latch assembly 10 and the associated door 8 in a closed condition. The claw 14 is in a closed position, retaining the striker (not shown). The pawl 16 is in an engaged position whereby the pawl tooth 40 is engaged with the closed abutment 34 , thereby holding the claw 14 in the closed position. The weather seals of the door 8 are in a compressed state, and the striker therefore generates a seal force FS on the mouth 32 of claw 14 , which tends to rotate the claw 14 in a clockwise direction when viewing FIG. 1 .
[0038] The seal force FS in turn generates a force FP onto the pawl tooth 40 and hence onto the pawl 16 . The force FP is reacted by the crank pin 54 of the crank shaft 50 . The force FP reacted by the crank pin 54 is arranged to produce a clockwise torque on the crank shaft 50 about the crank shaft axis A. However, the crank shaft assembly 18 is prevented from rotating clockwise when viewing FIG. 1 by virtue of the engagement between the release abutment 65 of the release lever 52 and the abutment 74 of the release plate 72 . The release plate 72 has been biased to the position shown in FIG. 1B by the spring 73 . Note that in the closed position, no electric current is flowing through electromagnet 71 , which accordingly exerts no magnetic force of the release plate 72 .
[0039] At the same time, the biasing lever 80 exerts a force FC on the claw 14 via the biasing pin 37 urging it into an open, released condition. A force FR on the reset lever 51 promotes the turning of the crank shaft 50 in a clockwise direction.
[0040] To release the latch assembly 10 , electric current is supplied to the electromagnet 71 , which creates a magnetic force which attracts the right hand end (when viewing FIG. 1B ) of the release plate 72 , causing the release plate 72 to rotate clockwise to the position shown in FIG. 2A . This in turn allows the release lever 52 and the crank shaft 50 to rotate clockwise (when viewing FIGS. 1 and 2 ) in an opening direction as a result of the force FP being reacted by the crank pin 54 and of the force FR.
[0041] Considering FIG. 1 , upon opening, the rotation of the crank shaft 50 is clockwise about the crank shaft axis A. The crank shaft axis A is defined by the cylindrical pin 56 being rotatably mounted in the retention plate 22 (as mentioned above) and the boss 61 being rotatably mounted in the backplate 24 (as mentioned above). Accordingly, the crank shaft axis A is fixed relative to the latch chassis 12 .
[0042] As mentioned above, when viewing FIGS. 1 and 2 , the forces FP and FR generate a clockwise torque upon the crank shaft 50 about the crank shaft axis A. Once the crank shaft 50 is freed to rotate (i.e., once the abutment 74 has disengaged from the release abutment 65 ), then the crank shaft 50 will move in a clockwise direction because the crank pin axis Y is constrained to move about an arc centred on the crank shaft axis A. Because the pawl pivot hole 46 is a close running fit on the crank pin 54 , a pawl axis Z (i.e., the center of the pawl pivot hole 46 ) is coincident with the crank pin axis Y. Accordingly, the pawl axis Z is similarly constrained to move about an arc centred on crank shaft axis A.
[0043] As the crank shaft 50 starts to rotate in a clockwise direction from the position shown in FIG. 1 , the claw 14 starts to open. The action of the claw 14 pushing on the pawl 16 and the biasing lever 80 pushing on the reset lever 51 causes the pawl 16 to move. As the pawl 16 moves, the angular position of the pawl 16 is controlled by engagement between the abutment surface 42 of the first arm 41 and the stop pin 29 , more particularly a contact point B defined between the abutment surface 42 and part of the cylindrical outer surface 29 A.
[0044] Generally speaking, the movement of the pawl 16 can be approximated to rotation about the contact point B (i.e., rotation about the contact point between the abutment surface 42 and the cylindrical outer surface 29 A). However, the movement is not truly rotational because a part of the pawl 16 (namely the pawl axis Z) is constrained to move about the crank shaft axis A rather than about the contact point B. Thus, the movement of the pawl 16 at the contact point B relative to the stop pin 29 is a combination of rotational movement and transitional (sliding) movement. Indeed, the contact point B is not stationary and will move a relatively small distance around the cylindrical outer surface 29 A and a relatively small distance along the abutment surface 42 . Thus, the contact point B is the position where (at the relevant time during opening of the latch assembly 10 ) the abutment surface 42 contacts the cylindrical outer surface 29 A.
[0045] Starting from the FIG. 2 position, once the abutment 74 has disengaged from the release abutment 65 , the force FR causes the biasing lever 80 to rotate clockwise about the biasing pin 37 (acting as a fulcrum), and the closed abutment 34 of the claw 14 pushes the pawl 16 (via the pawl tooth) to a position whereby the closed abutment 34 can pass under the pawl tooth 40 when viewing FIG. 3 . Once the pawl tooth 40 has thus disengaged from the closed abutment 34 of the claw 14 , the claw 14 is then free to rotate past the position shown in FIG. 3 to the fully open position as shown in FIG. 4 , urged in this direction by the forces FS and FC.
[0046] However, because the biasing pin 37 moves to the right, the biasing lever 80 pivots counter-clockwise about its pivotable connection with the reset lever 51 as it urges the claw 14 into the released position. At a predetermined point before or during this, the biasing lever nose 84 contacts the edge 60 A of the reset lever 51 . This may be before any rotation of the claw 14 has occurred (with contact occurring by virtue of the rotation of the crank shaft 50 alone) or once a certain amount of the claw 14 rotation has occurred.
[0047] As a result of a force FT acting on the edge 60 A, the direction in which the biasing lever 80 urges the reset lever 51 reverses so that it is now counter-clockwise about the crank shaft axis A as a fulcrum rather than clockwise. Thus, beyond this predetermined point, the biasing lever 80 acts to reset the crank shaft 50 to the position shown in FIG. 2 where it may re-engage the claw 14 and in which the release lever 52 rotates counter-clockwise back to the position shown in FIG. 1B in which it is retained by the release plate 72 . In other words, the crank pin axis Y resets to the FIG. 1 position, and the release lever 52 is returned to the FIG. 1B position.
[0048] As the reset lever 51 passes over the right hand end of release plate 72 , the release plate 72 is momentarily deflected and then snapped back into engagement (under the influence of the spring 73 ) such that the abutment 74 re-engages the release abutment 65 . Thus, when considering FIG. 4 , the pawl 16 , the crank shaft assembly 18 , and the release actuator assembly 20 are all in the same position as FIGS. 1 to 1 B. However, in FIG. 4 , the claw 14 is in the open position, whereas in FIGS. 1 to 1 B, the claw 14 is in the closed position.
[0049] Once the latch assembly 10 and associated door 8 has been opened, closing of the door 8 will automatically relatch the latch assembly 10 . Note however, that no rotation of the crank shaft 50 occurs during closing of the door 8 . Accordingly, the crank pin axis Y does not rotate, and the crank pin itself acts as a simple pivot having a fixed axis.
[0050] As mentioned above, the crank shaft assembly 18 is supported in a bearing of the retention plate 22 on one side of the crank pin 54 and is supported in a bearing in the backplate 24 on the other side of crank pin 54 . Thus, the crank shaft 50 is supported on both sides of the crank pin 54 , which is a particularly compact and strong arrangement. However, in further embodiments, the crank shaft 50 need only be supported on one side, i.e., the crank shaft 50 can be an overhung crank shaft 50 . An example of such an overhung crank shaft 50 would be provided by deleting the cylindrical pin 56 . Note that the crank shaft axis A would still be in exactly the same position because it would be defined by the cylindrical outer surface 62 .
[0051] The arrangement of the present invention permits a single biasing device (spring) to perform the function of promoting release and resetting of a crankshaft mounted pawl, while also urging a claw 14 into an open position.
[0052] The crank throw (the distance between the crank shaft axis A and the crank pin axis Y) is dimensioned, in this embodiment, such that no part of the cylindrical pin 56 sits outside the circumference of the crank pin 54 . This provides a particularly compact arrangement. In further embodiments, the crank pin axis Y can be offset from the crank shaft axis A by more than the radius of the crank pin 54 . In addition, suitable alternative biasing devices may be used in place of the torsion spring. The position at which the spring contacts the biasing lever 80 may be adjusted according to the proportion of the force required to be transmitted to the claw 14 and the reset lever 51 . The reset lever 51 could in alternative embodiments be integral with the crank shaft 50 . In addition, the reset lever 51 and the release lever 52 may be the same component. Furthermore, in a highly integrated design the crank shaft 50 , the reset lever 51 and the release lever 52 could all be a single component.
[0053] The foregoing description is only exemplary of the principles of the invention. Many modifications and variations are possible in light of the above teachings. It is, therefore, to be understood that within the scope of the appended claims, the invention may be practiced otherwise than using the example embodiments which have been specifically described. For that reason the following claims should be studied to determine the true scope and content of this invention. | A latch assembly includes a chassis and a rotatable claw-type latch bolt moveably mounted on the chassis. The latch bolt has a closed position for retaining a striker and an open position for releasing the striker. The latch bolt is provided with a latch abutment remote from a center of rotation. The latch assembly further includes a pawl rotatable about a pawl axis and having an engaged position for holding the latch bolt in the closed position and a disengaged position that allows the latch bolt to move to the open position. The latch assembly includes an eccentric arrangement defining a first axis and the pawl axis remote from the first axis. The latch assembly also includes a reset lever rotatably fixed to the eccentric arrangement for mutual rotation with the eccentric arrangement about the first axis. The latch assembly includes a biasing lever configured to transmit a biasing force to the reset lever at a position remote from the first axis and to the latch bolt via the latch abutment. The latch assembly includes a biasing device arranged to apply the biasing force to the biasing lever. The latch assembly is configured such that when the pawl retains the latch bolt in the closed position, the biasing lever applies a force to the reset lever to promote disengagement of the pawl, and such that when the pawl is disengaged, the biasing lever promotes the rotation of the latch bolt into the open position. | 4 |
BACKGROUND OF THE INVENTION
This invention relates to a process for controlling the final quality of synthetic polymeric yarns during manufacture thereof.
Conventionally, the quality of yarn is determined by taking final product yarn samples and measuring chemical and physical properties of the samples in the laboratory. One yarn property that is measured is relative viscosity of the yarn. The term "relative viscosity" as used herein is defined as the viscosity of a dilute solution of the polymer divided by the viscosity of the solvent employed. For polyamides, the standard measurement of relative viscosity is the viscosity of an 8.4 wt. % solution of the polyamide in a 90 wt. % formic acid solution divided by the viscosity of the 90 wt. % formic acid.
The laboratory measurement of relative viscosity may be used to make adjustments to process conditions if the relative viscosity measurements differ from desired relative viscosity levels. The disadvantage with this process is that the lag time between the laboratory measurement and the adjustments is generally too long to provide meaningful, effective control of the process.
U.S. Pat. No. 4,675,378 discloses a process control scheme for controlling the quality of a polymer by controlling melt viscosity. Control is effected by continuously measuring the melt viscosity at the outlet of the polymerization vessel. Operating conditions in the polymerization vessel are adjusted when the viscosity at this point strays from the pre-established level. Melt viscosity is also controlled by periodically measuring viscosity just before the spinneret. When this viscosity level deviates from a pre-set level, the pre-established viscosity level in the reaction vessel is adjusted.
It is believed that this process is inaccurate since it suffers from several disadvantages. One disadvantage is that inferring melt viscosity at finite locations such as at the exit of the polymerization vessel or at some point before the spinneret does not take into account changes that may take place in the material before it is actually formed into fibres.
Another disadvantage is that the pressure measurements taken by the viscometers of this process are taken close together. Pressure drops measured over short distances may give a good representation of the polymer viscosity at a precise location However, such pressure drops are typically relatively small, therefore the measurement of these pressure drops is less precise.
One approach that has been taken is to increase pressure drop and thus improve the accuracy of such viscometers. This may be done either by diverging a side stream of polymer through a smaller orifice or by increasing the flow rate of this side stream through the use of an additional pumping means. This approach may cause a number of problems. For example, the higher shear rates created by these methods of increasing the pressure may induce an increase in temperature. Also, at the required shear rate, the polymer may exhibit non-newtonian flow properties instead of newtonian flow properties, which may effect the reliability of the results.
It is an object of the present invention to obviate or mitigate the above-mentioned disadvantages.
Accordingly, the invention provides a process for controlling the relative viscosity of synthetic yarns during production thereof comprising the steps of:
taking at least three pressure measurements at three spaced locations in a transfer line for carrying molten polymer to a spinneret;
measuring temperature and throughput of polymer in said transfer line;
calculating an estimated relative viscosity of yarn produced by employing a predetermined correlation between pressure drop, throughput, temperature and relative viscosity; and
adjusting a meaningful operating condition in said melting zone in response to deviations in the estimated relative viscosity of said yarn from a desired relative viscosity of said yarn.
In another one of its aspects the invention provides a process for controlling the relative viscosity of synthetic yarns during production thereof comprising the steps of:
measuring the temperature and throughput of said yarn;
taking at least three pressure measurements at three spaced locations in a transfer line for carrying molten polymer to a spinneret;
calculating an estimated relative viscosity of yarn produced by employing the equation: ##EQU1## wherein: RV=relative viscosity
THPT=throughput of polymer
dP1=P1 - P2
dP2=P3 - P2
P1,P2,P3 pressure measurements taken ##EQU2## wherein:
Ea=activation energy for viscosity
R=ideal gas constant
T=absolute temperature of process
and
adjusting a meaningful operating condition in said melting zone in response to deviations in the estimated relative viscosity of said yarn from a desired relative viscosity of said yarn.
In another one of its aspects, the invention provides an apparatus for controlling the quality of yarn produced during manufacture thereof comprising:
at least three pressure sensors locatable within a transfer line for transferring molten polymer to a spinneret;
pressure measuring means and throughput measuring means associated with said transfer line for respectively measuring pressure and throughput of polymer therethrough;
calculation means for determining an estimated relative viscosity of said yarn employing a correlation between, temperature and throughput measurements made by said temperature measuring means and said throughput measuring means respectively, pressure measurements made by said pressure sensors and said estimated relative viscosity; and
control means associated with said calculation means for adjusting a meaningful operating condition in said polymerization vessel when said estimated relative viscosity deviates substantially from a desired relative viscosity of said yarn.
In the present invention, the relative viscosity of the yarn is estimated using a correlation that takes into account changes in polymer relative viscosity that may take place before the spinneret. A meaningful operating condition is then adjusted in response to any deviations in relative viscosity. The present invention thus allows for relatively accurate control of yarn relative viscosity.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention is particularly advantageous to use in yarn manufacturing processes wherein the polymer continues to react and/or change in the transfer line, since the present invention takes such changes into account by taking pressure measurements along the length of the transfer line and by extrapolating to determine RV of the yarn. The invention is most advantageously used with condensation polymers, which tend to undergo reaction with water in the transfer line. Most preferably, the polymer used is a polyamide or a polyester.
The meaningful operating condition controlled is preferably the water content of the polymer. In a unitary process, wherein polymer is made and then fed directly to the transfer line, the water content may be varied by employing a vacuum in the final polymerization vessel or finisher. In a split process, wherein pre-made polymer in the form of flakes or pellets is fed to an extruder and then travels to the transfer line, the water content may be varied by employing a vacuum in the extruder.
Preferably, the empirically determined constants in the correlation are calculated by measuring relative viscosity for known values of dP1 and dP2 and employing non-linear regression analysis. These constants are dependent on the flow properties of the polymer and the apparatus geometry. Thus if the apparatus geometry is changed, the constants may need to be recalculated. Also, these constants should be re-evaluated from time to time to ensure that internal apparatus geometry changes have not occurred due to gel formation.
The activation energy may be calculated empirically by varying temperature and measuring pressure variations or may be obtained from the literature.
The estimated relative viscosity is preferably determined at about one to ten minute intervals, and most preferably at about one minute intervals.
Preferred embodiments of the invention will be further described, by way of illustration only, with reference to the following figures in which:
FIG. 1 is a schematic representation of a batch yarn manufacturing process employing a process control system;
FIG. 2 is a schematic representation of a continuous yarn manufacturing process employing a process control system;
FIG. 3 is a graph of pressure versus distance along a transfer line.
FIGS. 4 is a graph of relative viscosity (RV) vs. time.
Referring to FIG. 1, it can be seen that in a split process, nylon flake is removed from a storage container 10 and is introduced through an inlet 12 into an extruder 14. Polymer melt extruded from the extruder 14 is then passed through a transfer line 16 to a spinneret 18. Located in this transfer line 16 in spaced relation to one another are three pressure gauges 20. These gauges are each electrically connected to a central control unit 22 which in turn is electrically connected to a valve 24 in a vacuum line 26 for creating a vacuum in the extruder 14.
In operation, the pressure gauges 20 measure pressure in the transfer line 16 and relay this information to the central control unit 22. This unit calculates an estimated relative viscosity and compares it to a desired final product viscosity. If the estimated value deviates from the desired value by a substantial amount, the central control unit 22 causes the valve in the vacuum line 24 to change its setting to change the amount of vacuum and hence the amount of water drawn out of the extruder.
In FIG. 2, it can be seen that in a unitary process, polymer is formed in a polymerizer, which may be a single vessel 28 as shown or a series of polymerization vessels. The polymer so formed is then sent to a final polymerization vessel known as a finisher 30. Polymer exiting from the finisher 30 is pumped by a pump 32 through a transfer line 34 to a spinneret 36. Located in this transfer line in spaced relation to one another are three pressure gauges 38. These gauges 38 are each electrically connected to a central control unit 40 which in turn is electrically connected to a valve 42 in a vacuum line 44 for creating a vacuum in the finisher 30.
In operation, the pressure gauges 38 measure pressure in the transfer line 34 and relay this information to the central control unit 40. This unit calculates an estimated relative viscosity and compares it to a desired final product viscosity. If the estimated value deviates from the desired value by a substantial amount, the central control unit 40 causes the valve 42 in the vacuum line 44 to change its setting to change the amount of water drawn out of the finisher.
The development of the correlation for use in the present invention is outlined below.
Expression for the Relative Viscosity, RV
The dependence of the melt viscosity on molecular weight, MW, has the following form:
n.sub.o =k MW.sup.a (1)
where a equals approximately 3.5 if MW is above a critical value and where n o is viscosity at a given reference temperature. For condensation polymers this value is quite low, of the order of about 5000 for the weight average molecular weight. The exponent a is therefore assumed to be 3.5 at all times.
The relation between RV and MW may be approximated by a linear relationship between RV and MW. This approximation is most accurate for RV values between 65 and 75, but will provide sufficiently accurate results for the range of RV values commonly associated with condensation polymers. It may therefore be assumed that RV and MW are proportional. From equation (1), it may be seen that RV depends on the melt viscosity raised to the power (1/3.5). The expression for melt viscosity has the following form
n.sub.o =dP/(Q * exp(-Ea/RT)) (2)
wherein Q is volumetric flowrate and dP is the pressure gradient.
By incorporating the relationship between M w and RV into equation (1), substituting the expression for n o of equation (1) into equation (2), and substituting throughput, THPT, for flowrate Q in equation (2) the following expression for RV is obtained: ##EQU3## wherein Tcorr is defined as a temperature correction factor and is equal to exp(-Ea/RT).
Pressure Drop at the Spinnerette
The required result of the calculations is RV at the spinneret. The term dP in expression (3) should thus represent the pressure gradient at the spinneret. It is necessary to use the three pressure measurements along the transfer line to extrapolate for the pressure gradient at the spinneret.
It is possible that the polymer coming into the transfer line may not have reached a final equilibrium RV value. In that case, changes in the MW of the polymer will still take place in the transfer line. There are three possible cases, assuming no change in geometry of the transfer line, which are illustrated in FIG. 3. If there is no change in RV along the transfer line, the pressure gradient remains constant, as illustrated by curve 50. Changes in the pressure gradient may arise from polymerization (curve 52) or depolymerization (curve 54) in the transfer line. In all three cases, the pressure, P, in the transfer line may be described by the expression:
P=A'x.sup.2 +B'x+C' (4)
where x is the linear distance in the transfer line and A', B', and C' are coefficients. The linear distances at which the pressure measurements are made need to be known if the coefficients are to be determined.
However, due to the presence of numerous friction generating elements in the line (i.e. elbows, motionless mixers, . . . ), the equivalent linear distances required in equation (4) may not be accurately evaluated. Thus an equation for RV not related to the linear distance is required.
If P 1 , P 2 , and P 3 are the three measured pressures, the pressure drops between two measurement points are given by:
dP.sub.1 =P.sub.3 -P.sub.2 =A'(x.sub.3.sup.2 -x.sub.2.sup.2)+B'(x.sub.3 -x.sub.2) (5)
dP.sub.2 =P.sub.2 -P.sub.1 =A'(x.sub.2.sup.2 -x.sub.1.sup.2)+B'(x.sub.2 -x.sub.1) (6)
The coefficients A' and B' from equations (5) and (6) may then be defined in the following way:
A'=[a(P.sub.3 -P.sub.2)+b(P.sub.2 -P.sub.1)]/c (7)
B'=[d(P.sub.3 -P.sub.2)+e(P.sub.2 -P.sub.1)]/f (8)
where the coefficients a, b, c, d, e, and f are combinations of x 1 , x 2 , and x 3 .
The pressure gradient at some position x 4 is obtained by differentiating equation (4): ##EQU4##
final expression
It has been shown in the last paragraph that the pressure gradient at some arbitrary position in the transfer line is proportional to a linear combination of two pressure drops. This allows for extrapolation of the pressure gradient at the spinning machine. The dP in equation (3) can therefore be replaced by a combination of dP 1 and dP 2 , the two measured pressure drops, to obtain the final expression: ##EQU5## where A, B, and C are empirical constants. These constants account for the intrinsic resistance to flow of the material as well as for the geometry of the assembly and the location of pressure measurements. They are therefore fixed for a given polymer and a given transfer line configuration and may be determined empirically.
These constants may be determined by measuring RV in the lab for known pressure drops and employing non-linear regression.
EXAMPLE 1
A process set up similar to that shown in FIG. 1 was used. Polymer temperature and throughput were measured. The activation energy was evaluated by varying temperature and measuring pressure variations. The constants A, B, and C were evaluated by measuring RV in the lab for known pressure measurements. The results of this are reported in Table 1.
The process was carried out for several days and RV was calculated daily using Equation (11). The calculated RV was compared to the measured RV. The results are shown in FIG. 4 which indicates that there is close agreement between calculated and measured RV.
TABLE 1______________________________________ EXPERIMENTALPARAMETER CONDITION OR RESULT______________________________________A -2.494E11B 3.138E11C -2.258E13Throughput (kg/hr.) 444-696Temperature (°C.) 288.4-291.6dP1 (psi) 126.5-264.2dP2 (psi) 291.9-584.9______________________________________ | A process for controlling the relative viscosity of synthetic yarns during production thereof. At least three pressure measurements are taken at three spaced locations in a transfer line for carrying molten polymer to a spinneret. Temperature and throughput of polymer in said transfer line are measured. An estimated relative viscosity of yarn produced by employing a predetermined correlation between pressure drop, throughput, temperature and relative viscosity is then calculated. A meaningful operating condition in the melting zone is adjusted in response to deviations in the estimated relative viscosity of said yarn from a desired relative viscosity of said yarn. | 3 |
TECHNICAL FIELD OF INVENTION
The invention relates to a process for the separation of the 2,6-diisopropylnaphthalene isomer from a feed stream of mixed isopropylnaphthalenes. A shape-selective adsorbant is employed resulting in a process that is more efficient than processes based upon prior separation techniques.
BACKGROUND OF THE INVENTION
The present invention relates to a process for separating 2,6-diisopropylnaphthalene from other isopropylnaphthalene isomers. The 2,6-diisopropyl isomer of naphthalene is of keen interest for the production of certain disubstituted aromatics which, in turn, are employed in the synthesis of liquid crystal polymers and specialty polyesters.
Such liquid crystal polymers and specialty polyesters would appear commercially attractive if either 2,6-dihydroxynaphthalene or 2,6-dicarboxynaphthalene were readily available. Unfortunately, these materials are not commercially produced because cheap, feed stocks do not exist. A viable feed stock which is convertible into either the dihydroxy or dicarboxy monomers, based upon known technology, is 2,6-diisopropylnaphthalene.
In any manufacture of diisopropylnaphthalene, it is clear that some monoisopropyl- and triisopropyl-products and a mix of diisopropyl isomers will also be obtained. In any crude diisopropylnaphthalene product which is not particularly enriched in the 2,6-diisopropylnaphthalene isomer, isomer separation by thermal distillation is very inefficient and difficult because the boiling points of 2,6-diisopropylnaphthalene and 2,7-diisopropylnaphthalene are very close. Similarly, 2,6-diisopropylnaphthalene separation by fractional crystallization using melting points is inefficient and suffers from yield problems because of the loss of the desired product in the mother liquor, and because of large recycled streams.
It is taught in U.K. patent application No. 2,199,590, filed on Nov. 27, 1987, that a specific isomer of dimethylnaphthalene can be separated from other isomers when a zeolite Y containing specific metallic ions is used as an adsorbant in combination with a specific desorbant. However, the adsorbant taught for use in the separation of the particular dimethylnaphthalene of the British reference would be of little value in isolating 2,6-diisopropylnaphthalene from other diisopropylnaphthalene isomers, since diisopropylnaphthalenes are larger molecules than dimethylnaphthalenes.
It is thus an object of the present invention to provide a selective adsorbant which has proven to be efficient in the selective adsorption of 2,6-diisopropylnaphthalene from a mixture of diisopropylnaphthalene compounds.
It is a further object of the invention to provide a process for enriching the fraction of 2,6-diisopropylnaphthalene contained in a feed stream of mixed dialkylated naphthalenes without engaging costly and inefficient distillation and crystallization techniques of the prior art.
It is still a further object of the present invention to provide a process for recovering substantially pure 2,6-diisopropylnaphthalene from a mixture of diisopropylnaphthalene isomers using selective adsorption in combination with conventional separation techniques such as fractional crystallization or distillation.
These and further objects will be more fully appreciated when considering the following disclosure and appended drawings wherein:
FIG. 1 represents a simulated moving bed column which can be employed in practicing the present invention; and
FIG. 2 is a graph demonstrating the efficacy of the present invention in illustrating ratios of 2,6-diisopropylnaphthalene adsorbed with the volume of desorbant employed.
SUMMARY OF THE INVENTION
The present invention is both to a shape selective adsorbant for the selective adsorption of 2,6-diisopropylnaphthalene from a feed stream of mixed diisopropylnaphthalenes as well as to a process for separating the 2,6-diisopropyl isomer from a mixture of isomers of diisopropylnaphthalenes. It was discovered that the optimum shape selective adsorbant is a class of crystalline molecular sieves all of which are characterized as having 12 member oxygen rings and pore aperture dimensions between approximately 5.5Å and 7.0Å. The process involves contacting a quantity of mixed diisopropylnaphthalene isomers with an adsorbant bed containing one or more of the above crystalline molecular sieves.
Following the adsorption step, the material held up in the interstices is removed. At this point, the bed contains sorbed material that is rich in 2,6-diisopropylnaphthylene. The material sorbed by the bed is then displaced from the bed with a suitable desorbant. The desorbant can then be separated from the desorbed diisopropylnaphthalenes and recycled. The product is a material rich in 2,6-diisopropylnaphthalene. If desired, this enriched material can be further purified by any of several means including, for example, distillation, crystallization, or a second absorption step.
DETAILED DESCRIPTION OF THE INVENTION
As noted previously, the present invention is both to a shape selective adsorbant for the selective adsorption of 2,6-diisopropylnaphthalene from a feed stream of mixed diisopropylnaphthalenes as well as to a process for separating the 2,6-diisopropyl isomer from a mixture of isomers of diisopropylnaphthalenes. This can be done as a batch process while establishing a unit operation by moving the feed stream of mixed isomers over a bed of suitable adsorbant. This is conducive to commercializing the present process, for large quantities of mixed dialkylated naphthalene isomers can be processed in such a unit operation. The present process can be carried out employing, for example, chemical processing equipment used previously for such things as liquid bulk separations. For example, FIG. 1 illustrates a schematic representation of such bulk separation equipment as employed by UOP for the adsorptive separation of p-dialkylbenzene from other dialkylbenzene isomers. See D. B. Broughton, "Bulk Separations Via Adsorptions", Chemical Engineering Progress, pp. 49-51 (October, 1977). However, it must be emphasized that virtually any well known packed column can be employed insuring a flow of liquid feed stock and desorbant over a fixed bed of adsorbant which can be employed as a powder, pellet, or extrudate.
Referring to FIG. 1, the preferred process utilizes a column 2 filled with a fixed bed of adsorbant. The column has numerous ports 4 for feeding dialkylnaphthalene feed and desorbant as well as removing raffinate and extract. These ports are all piped to a rotary valve 8 which controls where in the adsorption column materials are fed and withdrawn. For a period of time, dialkylnaphthalene feed is provided to a section of the adsorption column wherein the adsorbant selectively adsorbs the desired 2,6-diisopropylnaphthalene isomer. The raffinate now depleted in the desired 2,6-diisopropylnaphthalene isomer is either recycled by pump 6 or withdrawn and sent to a column 10 where any desorbant it picks up is separated and returned. At a later period in time, the rotary valve 8 redirects the stream and now desorbant is fed over the portion of the packed bed which had previously adsorbed the desired 2,6-diisopropylnaphthalene isomer. The desorbant releases the desired isomer (the extract) from the adsorbant and passes through the rotary valve to a column 12 in which 2,6-diisopropylnaphthalene is separated from the desorbant.
If the 2,6-diisopropylnaphthalene enriched product does not contain sufficient purity of the desired isomer, it can be further purified by another adsorption step, fractional crystallization, or other conventional separation means.
The adsorbants employed for the preferential removal of the 2,6-diisopropyl isomer from a feed stock of mixed dialkylated naphthalenes are one or more crystalline molecular sieves such as those taught in Applicants' co-pending U.S. application Ser. No. 254,284, filed on Oct. 5, 1988, entitled SELECTIVE ISOPROPYLATION OF NAPHTHALENES TO 2,6-DIISOPROPYLNAPHTHALENES, the disclosure of which is hereby incorporated by reference. Broadly, the adsorbants of the present invention for the selective adsorption of 2,6-diisopropylnaphthalene from other diisopropylnaphthalene isomers are crystalline molecular sieves containing 12 membered oxygen rings and pore aperture dimensions between approximately 5.5Å and 7.0Å.
Shape selective adsorption occurs when the zeolite framework and its pore structure allow molecules of a given size and shape to preferentially diffuse into and adsorb within the intracrystalline free space. It is therefore important to characterize accurately the pore structure that is encountered in the various crystalline molecular sieve frameworks. Pore structure (dimensions and network) varies greatly among zeolites. Without modifications of the zeolite structure, the lowest pore aperture dimension is about 2.6Å and the highest is 7.4Å. Maximum values for the four-, six-, eight-, ten-, and twelve-membered oxygen rings have been calculated to be 2.6 Å, 3.6 Å, 4.2 Å, 6.3 Å, and 7.4 Å, respectively. Pores may lead to linear, parallel, or interconnected channels or may give access to larger intracrystalline cavities, sometimes referred to as cages. For all zeolites, the pore opening is determined by the free aperture of the oxygen ring that limits the pore aperture.
The free diameter values given in the channel description and on the ring drawings (not shown here) are based upon the atomic coordinates of the type species in the hydrated state and an oxygen radius of 1.35 Å, as determined from x-ray crystallographic data. Both minimum and maximum values are given for noncircular apertures. In some instances, the corresponding interatomic distance vectors are only approximately coplanar; in other cases the plane of the ring is not normal to the direction of the channel. Close inspection of the framework and ring drawings should provide qualitative evidence of these factors. Some ring openings are defined by a very complex arrangement of oxygen atoms. Included are references to publications which contain extensive drawings and characterization data. The relevant portions of those references are incorporated herein. It should be noted that crystallographic free diameters may depend upon the hydration state of the zeolite particularly for the more flexible frameworks. It should also be borne in mind that effective free diameters can be temperature dependent.
As used throughout the instant specification, the term "pore aperture" is intended to refer to both the pore mouth at the external surface of the crystalline structure, and to the intracrystalline channel, exclusive of cages. When a crystalline molecular sieve is hereinafter characterized by a "pore aperture dimension," adopted is the geometric dimensional analysis defined as ♭crystallographic free diameter of channels" in Meier, W. M., Olson, D. H., Atlas of Zeolite Structure Types, (Butterworth's, 1987, 2d Rev. Ed.). The term "dimension" is preferred over "diameter" because the latter term implies a circular opening, which is not always accurate in crystalline molecular sieves.
Crystalline molecular sieves which are useful in practicing the present process include MeAPSO-46, offretite, ZSM-12 and synthetic mordenite. Preferred adsorbants are synthetic mordenite, with pore aperture dimensions of 6.5 Å and 7.0 Å and ZSM-12 with pore aperture dimensions of 6.2 Å, 5.7 Å and 5.5 Å. These preferred adsorbants can be used in the adsorption process without any pretreatment to modify their pore aperture dimensions. Synthetic mordenite is particularly preferred while other useful adsorbents may be obtained by treatment of an acidic crystalline molecular sieve having pore aperture dimensions greater than 7.0 Å selected from the group consisting of zeolite L, zeolite Beta, faujasite and SAPO-5 to reduce the dimensions of the pore apertures. Mordenite, ZSM-12, offretite and MeASPO-46 fall into the first class of adsorbants whose pore aperture dimensions are between 5.5 Å and 7.0 Å, prior to any modification to their pores.
The preferred adsorbants, mordenite and ZSM-12, as well as other suitable sieves, can be optimized to greater selective adsorption of the desired 2,6-diisopropylnaphthalene without substantially altering their pore dimensions by modifying the hydrophobic character of the molecular sieves. One such modification to the preferred adsorbants is to dealuminate. Dealumination of acidic crystalline molecular sieve materials can be achieved by exposing the molecular sieve to mineral acids such as HCl. The desired degree of dealumination will dictate the strength of acid used and the time during which the crystalline structure is exposed to the acid. It is also common to use a steam treatment in combination with the acid leach to dealuminate the zeolite materials. For additional methods of preparing aluminum-deficient zeolites, see J. Scherzer, "The Preparation and Characterization of Aluminum-Deficient Zeolites", Thaddeus E. Whyte et al., "Catalytic Materials: Relationship Between Structure and Reactivity", ACS Symposium Series 248, pp. 156-60 (American Chemical Society, 1984). Dealumination according to the instant invention is intended to achieve a Si:Al ratio above 3 and preferably above 15. Dealumination can also be applied to the second class of molecular sieve materials whose pore aperture dimensions exceed 7.0 Å.
A dealuminated crystalline molecular sieve can be calcined at temperatures between 400° C. and 1000° C., preferably between 400° C. and 600° C. Calcination serves to dehydrate or "heal" Si-OH bonds or "nests" after dealumination. Healing these nests provides for a more uniform pore structure within the crystalline material, leading to structural stability and ultimately resulting in improved adsorption. For a zeolite like hydrogen mordenite, the optimal temperature range was found experimentally to lie between 400° C. and 600° C., but preferentially at 500° C. See Mathur, Kuldeep, Narain, Ph.D. Thesis, University of Pittsburgh, 1977. In the case of H-mordenite, removal of extra and intra crystalline water can be accomplished effectively in the presence of an atmosphere of oxygen or nitrogen.
As previously noted, other adsorbants may also be considered which have aperture dimensions in excess of 7.0 Å. These other adsorbants are obtained by a combination of modifications of commercially available, acidic crystalline molecular sieve products. Examples of such sieves include zeolite L, zeolite Beta, faujasite and SAPO-5, which have 12 membered oxygen rings whose pore aperture dimensions typically exceed 7.0 Å. SAPO is an acronym for silicoaluminophosphate molecular sieves, first reported in 1984. See U.S. Pat. No. 4,440,871 to B. M. Lok et al. MeAPO is an acronym for metalaluminophosphate molecular sieves reported in U.S. Pat. No. 4,567,029 to S. T. Wilson et al. For more complete characterizations of each of the catalyst members discussed above, see Flanigen, E. M., et al., Stud. Surf. Sci. Cat., 28, pp. 103-12. Also, see E. G. Derouane, "Diffusion and Shape-Selective Catalysis in Zeolites", Intercalation Chemistry, pp. 112-14, Ed. by M. Stanley Whittingham (Academy Press, 1982). Also, see S. Ernst, Zeolites, Vol. VII, p. 458 (1987 ), for a good discussion of ZSM-12.
When using adsorbants obtained by the treatment of crystalline molecular sieves whose pore aperture dimensions are initially above 7.0 Å, internal acid site modification can be used to reduce the pore aperture dimensions to an extent which show an enhanced 2,6-diisopropylnaphthalene selectivity. Molecular sieves with reduced port aperture dimensions are best described with reference to their performance in the adsorption under consideration. Those crystalline molecular sieves which have been adequately modified by internal acid site treatment will perform the selective adsorption of 2,6-diisopropylnaphthalene.
Ion exchange can be used to treat crystalline molecular sieves whose pore aperture dimensions are initially above 7.0 Å and reduce the pore aperture to the desired range. Elements suitable for ion exchange include alkali metals and alkali earth metals.
Crystalline molecular sieves may be treated to modify internal acid sites by contact with reagents selected from the group consisting of halogen, hydridic and organic derivatives of group 3A, 4A, 4B and 5A. Preferred embodiments of the internal acid site reagents include B 2 H 6 , SiH 4 and PH 3 . For a more complete discussion of the internal acid site modification techniques contemplated herein, see A. Thijs et al., J. Chem. Soc. Faraday Trans., 79, 2821 (1983). See also J. Philippaerts et al., "The Implantation of Boron-Nitrogen Compounds in Mordenite LP and Their Influence on the Adsorption Properties", Stud. Surf. Sci. Catal., 28, pp. 305-10 (1986). The relevant portions of each of these citations are incorporated herein by reference.
In addition to the use of the above-described reagents which tend to be nonspecific, there is an intermediate level of crystalline molecular sieve modification which can be used to perform "pore mouth engineering". These reagents provide an intermediate level since they are not specific for external acid site, but are not entirely nonspecific, leading to substantial internal acid site modification. In selecting an intermediate reagent, the characteristics and pore aperture dimensions of the starting crystalline molecular sieve must be matched against the molecular dimensions of the reagent.
It has been shown that chemical vapor deposition of Si(OCH 3 ) 4 on H-mordenite can be successfully used to control the intracrystalline pore aperture without substantially affecting the adsorbant's internal surface acid properties. Si(OCH 3 ) 4 can be deposited irreversibly on zeolite without entering the intracrystalline pores. See Niwa, M. et al., J. Chem. Soc., Faraday Trans., 1, 1984, 80, pp. 3135-45; Niwa, M. et al., "Modification of H-Mordenite by Vapor-Phase Deposition Method", J. Chem. Soc. Commun., p. 819-20 (1982).
Similarly, chemical vapor deposition of metal chlorides such as SiCl 4 , GeCl 4 , TiCl 4 , and SnCl 4 can be effective to modify pore mouth structures. These metal molecules with a range of molecular dimensions can be selected to be larger than the adsorbant pore aperture, thereby preventing substantial diffusion into the internal pore. See Hidalgo, T. V. et al., Zeolites, 4, pp. 175-80 (April, 1984).
The pore-modifying agents can be contacted with the molecular sieves in either solution or in vapor phase.
As noted previously, the crystalline molecular sieve adsorbant can be supplied as a powder, pellet or extrudate. Pellets and extrudates can be made according to known techniques for binding power. Pellets can be formed by applying pressure to powder. Pellets and extrudates can be formed by using binders such as alumina, clays, silica, or can be silica-alumina as well known in the art. In one embodiment of the process, the adsorbant is packed in a column and a stream of mixed diisopropylnaphthenes pass through the column. After a suitable contact time with the adsorbant bed, the depleted dialkylnaphthalene stream is purged from the packed bed. In a second step, a desorbant is fed to the column to remove the adsorbed isomers. The stream containing the desorbant and the adsorbed isomers is collected. The dialkylate fraction of this stream which is enriched in 2,6-diisopropylnaphthalene, can be separated from the desorbant by any conventional separation means such as by crystallization, thermal distillation or chromatographic adsorption. It is also contemplated that a series of adsorption/desorption cycles can be employed.
The desorbant is a liquid chosen to selectively desorb the isomers absorbed by the adsorbant. The desorbant is also chosen as a material which is easily and efficiently separated from the desired 2,6-diisopropyl isomer. In this regard, it was found that various alcohols, ethers, single ring alkylaromatics such as p-xylene and o-xylene are particularly preferred while other desorbants contemplated for use herein include m-xylene, toluene, ethylbenzene, n-propylbenzene, isopropylbenzene, 4-ethyltoluene, 1,2,4-trimethylbenzene, p-diethylbenzene, p-cymene, 1,2,3,4-tetrahydronaphthalene and mixtures thereof.
The temperature and pressure conditions for the adsorption process also affect the diffusion rate. The temperature must be between ambient and 300° C., preferably between 100° C. and 200° C. The pressure in the packed column must be between 0 psia and 5000 psia, preferably about atmospheric pressure but in any case higher than the vapor pressure of the alkylnaphthalene feed at the temperature of the adsorption step.
EXAMPLE 1
A 1/4 inch O. D. stainless steel tube 12 inches long was packed with a steam de-aluminated, acid washed and calcined mordenite powder (381-10, Si/Al=23). The column was heated to a temperature of 104°-119° C. and a sample of a dialkylnaphthalene stream was pumped over the bed at a rate of 0.25 ml/min. Analysis of the initial liquid exiting the column showed a depletion of 2,6-diisopropylnaphthalene isomer over that contained in the feed stream (Table 1).
TABLE 1______________________________________Total Initial Ratio Final RatioIsomer/DIPN's (% by Wt.) (% by Wt.)______________________________________2,6 18.8 4.92,7 15.8 10.71,3 20.6 30.11,5 4.0 3.81,4 8.1 11.31,6 17.0 24.31,7 14.2 12.8TOTAL 98.5 97.92,6/2,7-DIPN 1.2 0.5______________________________________
These data show that the 2,6-diisopropylnaphthalene isomer was preferentially removed from the dialkylnaphthalene stream since the 2,6/2,7 ratio dropped from 1.2 to 0.5. Also the percentage of the 2,6-diisopropyl isomer changed from 18.8 to 4.9% further illustrating the selection of this isomer by the adsorbant.
EXAMPLE 2
The mordenite sieve used in Example 1 was loaded into a 1/4 inch diameter stainless steel tube 12 inches long. A mixture of diisopropylnaphthalene was pumped over ca. 1.8 gm of the sieve at 157° C. at 0.25 ml/min. Samples of the dialkylnaphthalenes passing over the mordenite bed were collected at 0.5 ml increments. Table 2 shows the mole % composition of the dialkylnaphthalene stream fed to the column. The initial 2,6/2,7 ratio was 1.19. Table 3 shows the 2,6/2,7 ratio for the samples collected after contact with the mordenite. The data shows that the 2,6/2,7 ratio dropped from 1.19 to 0.5 after 4.3 were pumped.
TABLE 2______________________________________Mole % Composition of DIPN Isomer mol %______________________________________ 2,6 18.8 2,7 15.8 1,3 20.6 1,5 4.0 1,4 8.1 1,6 17.0 1,7 14.2______________________________________
TABLE 3______________________________________2,6/2,7 Ratio of Adsorbed DIPNvolume pumped (ml) 2,6/2,7______________________________________4.3 0.505.0 1.137.0 1.179.5 1.19______________________________________
After pumping 9.5 ml of dialkylnaphthalene, the 2,6/2,7 ratio finally reached the initial value. After the 2,6/2,7 ratio was at the initial value of 1.19 the dialkylnaphthalene feed stream was turned off and p-xylene was pumped to flush the adsorbed 2,6-diisopropylnaphthalene from the sieve. FIG. 2 shows the ratio of the 2,6-diisopropyl isomer/total dialkylated naphthalenes as a function of the amount of xylene pumped. From the graph it can be seen that the first material eluted is probably the original dialkylate displaced from the void space between the mordenite particles, since the 2,6/total isomers is 0.2 (or 20%) initially. The maximum in the curve is due to the 2,6-isomer being displaced from the pore of the sieve. The enrichment is significant since the sample taken at 6.8 ml contains 54% 2,6-DIPN as compared to 19% in the initial dialkylate mixture. | A process for enriching the fraction of 2,6-diisopropylnaphthalene contained in a quantity of mixed dialkylated naphthalenes. The mixed dialkylated naphthalenes are contacted with an adsorbant bed containing one or more molecular sieves which demonstrate shape selective preference for the 2,6-diisopropylnaphthalene isomer over other dialkylated naphthalenes. The adsorbant bed is then contacted with a desorbant capable of desorbing the 2,6-diisopropylnaphthalene from the pores of the adsorbant. | 2 |
CROSS REFERENCE TO RELATED APPLICATION
This application is a divisional of U.S. patent application Ser. No. 10/853,601, filed on May 25, 2004, now U.S. Pat. No. 7,464,543, which is hereby incorporated by reference.
FIELD OF THE INVENTION
The present invention relates to a silencer/catalytic converter unit for use with an internal combustion engine, in particular to a two-stroke lean burn internal combustion engine using a normally gaseous hydrocarbon as fuel. The present invention further relates to a two-stroke engine incorporating the silencer/catalytic converter unit. Additionally, the present invention relates to a method for converting an existing 2-stroke engine to a low emissions 2-stroke engine. Finally, the present invention relates to a method for reducing carbon monoxide, formaldehyde and volatile organic compounds (VOC) emissions in the exhaust of a 2-stroke natural gas fueled engine.
BACKGROUND OF THE INVENTION
Two-stroke (alternatively referred to as two-cycle) engines have been known for many years and have been applied in a range of applications. One class of two-stroke engines is the class of engines operating on a normally gaseous hydrocarbon, most commonly natural gas, under lean burn conditions. Such engines are generally large, slow running engines of a stationary design and find application in the driving of rotating and reciprocating equipment, such as compressors and electric generators. One example of commercially available engines is the Ajax® series of engines manufactured and sold by the Cooper Energy Services division of Cooper Cameron Corporation. The Ajax engines are two-stroke engines having from one to four cylinders. When used to drive a compressor, the Ajax engines are commonly employed in a configuration in which the cylinders of a reciprocating compressor are driven from the same crankshaft as the cylinders of the engine.
Engines of this class generally operate at low speeds, that is speeds of the order of from several hundred to a thousand revolutions per minute. The engines are generally operated in a constant speed mode, in which a substantially constant speed is maintained under a variety of engine loads. As the power demand placed on the engine is increased, the combustion efficiency and performance of the engine improves.
Recent environmental regulations have been increasing the emphasis on the importance of reducing the levels of partially burned fuel constituents from the exhaust of stationary engines. These regulated exhaust emissions consist of CO, NMHC, and formaldehyde (CH 2 O). An oxidizing catalyst in the exhaust stream will produce dramatic reductions in the levels of these emissions. Accordingly, there is a need for a way to reduce carbon monoxide, formaldehyde and volatile organic compounds (VOC) emissions from engines in this class.
One method of reducing the amount of such emissions in other types of internal combustion engines is to employ a catalytic converter in the exhaust system of the engine. The catalytic converter converts such emissions in the exhaust gases to less harmful emissions before they are emitted to the atmosphere. However, that has proven more difficult in practice. Previous industry experience with applying oxidizing converters to 4-stroke natural gas fueled engines indicates satisfactory results relative to the removal efficiencies of the subject emissions and the duration of operating time accumulated between catalyst cleaning and/or element replacement. However, previous tests of oxidizing catalysts with 2-stroke natural gas fueled engines have demonstrated good removal efficiencies for only short time periods. Therefore, currently available lean burn catalyst systems are limited to 4-stroke engine applications.
The majority of oxidation catalysts use a combination of platinum (Pt), rhodium (Rh), and palladium (Pd). Under the lean conditions that these engines are run, there is excess oxygen present in the exhaust. With excess oxygen present, oxidation catalysts are effective at eliminating carbon monoxide, formaldehyde and VOC emissions.
All of the chemical reactions that occur in a catalyst occur at the surface. So, any decrease in the surface area or the number of active sites available of the catalyst results in a decrease in the effectiveness of the catalyst. The specific deactivation mechanisms present in 2-stroke lean burn natural gas engines include selective poisoning and non-selective poisoning.
Selective poisoning occurs when a material reacts directly with the catalytic material rendering it unable to function as a catalyst. Poisoning is generally a reversible process, which is treated by using heat, washing or simply removing the poison from the exhaust stream. Sulfur from engine oil in the exhaust stream is a major contributor to catalyst poisoning.
Non-selective poisoning is also referred to as masking or fouling. It is the result of materials in the exhaust flow that accumulate on the catalyst surface. Phosphorous compounds and other materials, which are common in lubricating oils and in partially burned combustion products, can be found on the surface of the catalyst.
Differences in catalyst performance are also affected by temperature. Higher temperatures increase catalyst efficiency and may impede poisoning. The difference in temperatures is why 4-stroke natural gas fueled engines have been successfully outfitted with catalytic converters and why there is still a need for them in 2-stroke natural gas fueled engines. The difference in temperatures is due to the differences in engine design. Because of the scavenging process, 2-stroke engines have cooler exhaust temperatures than 4-stroke engines that consequently hinder exhaust performance.
M. DeFoort et al. of Colorado State University reported these problems and differences at the Gas Machinery Conference 2002 in Nashville, Tenn. on Oct. 8, 2002, in their paper entitled Performance Evaluation of Oxidation Catalysts for Natural Gas Reciprocating Engines. This paper discloses the use of a catalyst in an attempt to treat the exhausts from 2-stroke and 4-stroke lean burn natural gas fueled engines. The catalyst efficiency dropped from 95% to 80% for CO and from 75% to 45% for formaldehyde during the catalyst aging process for a large bore 2-stroke engine (about 200 hours). However, the results for the medium bore 4-stroke engine were better due to the nearly 200 degree F. higher catalyst temperatures. The catalyst efficiency dropped from 99.2% to 97.7% for CO and from essentially 100% to 67% for formaldehyde during the catalyst aging process (about 150 hours).
The specific 2-stroke engine used was a Cooper-Bessemer GMV-4TF stationary internal combustion engine having four cylinders with a manufacturer's sea level rating of 440 brake-horsepower (bhp) at 300 rpm. The cylinders were 14 inches in diameter with a 14-inch stroke. Air was delivered to the engine using a supercharged air delivery system. During the scavenging process, about half of the air supplied to the engine passed through the engine and was not trapped in the cylinder. The other half of the supplied air was trapped in the cylinder and participated in the combustion process. The catalyst was contained in a housing having four units, each measuring 12″×16″×3″. The housing was inserted in the exhaust line, but its location is not clear from the article since FIG. 6.1 showing its location was not published with the article.
M. DeFoort et al. analyzed the catalyst used with the 2-stroke engine. They found that the leading edge of the catalyst had three oxides not present in the trailing edge of the catalyst. These were oxides formed from copper (CuO), phosphorus (P 2 O 5 ) and zinc (ZnO). Sulfur also played a role in the deterioration of the catalyst. The elements copper, phosphorus and zinc, plus other elements such as iron and calcium, contributed to the deactivation of the catalyst, all of which are known catalyst poisons originating from engine lubricants and coolants. In addition, black soot was found on the leading edge of the catalyst.
In summary, M. DeFoort et al. concluded based on their results that oxidation catalysts were not likely to be effective for large bore 2-stroke lean burn engines. The oxidation catalyst showed clear signs of poisoning in a relatively short period of time (less than 250 hours) when compared to the expected lifespan of the catalyst.
While catalytic converters for a 2-stroke engine are known in the art, their application has been limited to 2-stroke engines of much smaller capacity and operating at speeds far greater than those of the class of engines addressed by the present invention. See, for example, catalytic converters disclosed in U.S. Pat. No. 6,277,784 (for small engines); and muffler/catalytic converter combinations disclosed in U.S. Pat. No. 4,867,270 (for portable hand tools); U.S. Pat. No. 5,866,859 (for portable work tools); U.S. Pat. No. 5,916,128 (for small 2-stroke engine); U.S. Pat. No. 6,109,026 (for portable work tools); U.S. Pat. No. 6,315,076 (for small engines); U.S. Pat. No. 6,403,039 (for small engines); and U.S. Pat. No. 6,622,482 (for small engine applications).
To date because of the problems noted by M. DeFoort et al., such catalytic converter exhaust systems have not been applied to large capacity 2-stroke lean burn engines operating on a normally gaseous hydrocarbon fuel and operating at speeds at or below about 1000 rpm.
Accordingly, there is a need for a solution to the problem of achieving lower carbon monoxide and formaldehyde emissions in the exhaust from large capacity 2-stroke lean burn engines operating on a normally gaseous hydrocarbon fuel and operating at speeds at or below about 1000 rpm, while maintaining a satisfactory level of catalyst efficiency and requiring little maintenance over and above the existing maintenance schedules.
SUMMARY OF THE INVENTION
Accordingly, the present invention satisfies this need by broadly providing a combination exhaust silencer and oxidizing catalytic converter unit applied to a large capacity two stroke, lean burn (2SLB), gaseous fueled engine operating at speeds at or below about 1000 rpm and utilizing a lubricating oil with a zinc content of at most 10 ppm and which preferably has a very low ash content (less than 0.1 wt %).
In one aspect of the invention, there is provided a low emissions 2-stroke natural gas fueled engine. The engine includes at least one cylinder with an inlet port and an exhaust port, and a silencer/catalytic converter unit, wherein the exhaust port in communication with the silencer/converter. In one embodiment, an exhaust line is connected at one end to the exhaust port and at the other end to the silencer/converter unit, thereby placing the exhaust port in communication with the silencer/converter. In another embodiment, an exhaust line is connected at one end to the exhaust port and at the other end to an exhaust manifold with the silencer/converter unit connected to an exhaust manifold, thereby placing the exhaust port in communication with the silencer/converter. The silencer/catalytic converter unit comprises a first volume and a second volume; wherein the first volume and the second volume are in communication with each other. The first volume is for dampening spurious exhaust pressure excursions and for removing at least a portion of the particulates contained in an untreated engine exhaust. The first volume can be one or more chambers. The second volume houses an oxidation catalyst for reducing emissions in a treated engine exhaust below the emissions in the untreated engine exhaust. The engine also has a lubricating engine oil having a zinc content of at most 10 ppm, thereby reducing the metal poisons contained in the untreated exhaust prior to contact with the oxidation catalyst. Preferably, the lubricating engine oil has a zinc content of at most 5 ppm. The lubricating engine oil is preferably produces very low ash, thereby minimizing the amount of sulfur combustion components contained in the untreated engine exhaust to reduce masking of the oxidation catalyst. The first volume preferably has a pressure relief valve set to relieve at a pressure greater than the maximum normal operating pressure of the engine to avoid excessive pressure excursions of the engine exhaust from damaging the oxidation catalyst.
In another aspect of the invention, there is provided a method for converting an original 2-stroke natural gas fueled engine to a converted 2-stroke natural gas fueled engine having lower emissions. The method comprises providing the original 2-stroke natural gas fueled engine producing an untreated engine exhaust containing particulates. The original engine has at least one or more cylinders with an inlet port and an exhaust port, a silencer in communication with the exhaust port; and an unmodified lubricating engine oil having a zinc content of at least 300 ppm. The method also includes replacing the silencer with a silencer/catalytic converter unit. The silencer/catalytic converter unit includes a first volume for dampening spurious exhaust pressure excursions and removing at least a portion of the particulates contained in the untreated engine exhaust, and a second volume housing an oxidation catalyst for reducing emissions in a treated engine exhaust below the emissions contained in the untreated engine exhaust, wherein the first volume and the second volume are in communication with each other. The method further includes positioning the oxidation catalyst within the second chamber such that the untreated engine exhaust has a temperature of at least 600 degrees F.; and replacing the unmodified lubricating engine oil with a low metals lubricating engine oil having a zinc content of at most 10 ppm, more preferably at most 5 ppm, thereby reducing the metal poisons contained in the untreated engine exhaust prior to contact with the oxidation catalyst. Preferably, this method also includes the step of installing a pressure relief valve in the first volume set to relieve at a pressure greater than the maximum normal operating pressure of the engine to avoid excessive pressure excursions of the engine exhaust from damaging the oxidation catalyst. The low metals lubricating engine oil preferably produces a very low ash content (less than 0.1 wt %), thereby minimizing the amount of sulfur combustion components contained in the untreated engine exhaust to reduce masking of the oxidation catalyst.
In yet another aspect of the present invention, there is provided a method for reducing carbon monoxide, formaldehyde and VOC emissions in the exhaust of a 2-stroke natural gas fueled engine. The method includes lubricating said engine with a lubricating engine oil composition having a zinc content of at most 10 ppm, more preferably at most 5 ppm; feeding an untreated engine exhaust of the engine to a silencer/converter to produce a treated engine exhaust; and positioning the oxidation catalyst within the second chamber such that the untreated engine exhaust has a temperature of at least 600 degrees F. The silencer/converter has at least a first volume for dampening spurious exhaust pressure excursions and removing at least a portion of the particulates contained in the untreated engine exhaust, and a second volume housing an oxidation catalyst for reducing emissions in the treated engine exhaust below the emissions in the untreated engine exhaust. The first volume and the second volume are in communication with each other. The lubricating engine oil utilized herein preferably produces very low ash (less than 0.1 wt %), thereby minimizing the amount of sulfur combustion components contained in the untreated engine exhaust to reduce masking of the oxidation catalyst. Preferably, the method includes the further step of installing a pressure relief valve in communication with the first volume set to relieve at a pressure greater than the maximum normal operating pressure of the engine to avoid excessive pressure excursions of the engine exhaust from damaging the oxidation catalyst.
In further aspect of the present invention, there is provided a silencer/catalytic converter unit for a 2-stroke natural gas fueled engine. The silencer/catalytic converter unit includes an oxidation catalyst for reducing carbon monoxide and formaldehyde emissions in an untreated engine exhaust; a first volume for dampening spurious exhaust pressure excursions and removing at least a portion of the particulates contained in the untreated engine exhaust; a second volume housing the oxidation catalyst for reducing emissions in a treated engine exhaust below the emissions in the untreated engine exhaust; and a pressure relief valve in communication with the first volume set to relieve at a pressure greater than the maximum normal operating pressure of the engine exhaust to avoid excessive pressure excursions of the engine exhaust from damaging the oxidation catalyst. The first volume and the second volume are in communication with each other. The oxidation catalyst is positioned within the second chamber such that during operation of the engine the untreated engine exhaust has a temperature of at least 600 degrees F. at that position. Preferably, at least one exhaust flow pipe provides the communication between the first and second volumes. Each of the at least one exhaust flow pipes has a catalyst facing end which is closest to the first catalyst face of the oxidation catalyst. The distance between the catalyst facing end and the first catalyst face is sufficient to provide a substantially uniform flow of the untreated exhaust upon contact across the first catalyst face during engine operation. This enhances the utilization of the oxidation catalyst.
Catalyst:
The oxidation catalyst reduces the concentration of carbon monoxide, formaldehyde and VOC's in the engine exhaust. Such catalysts are commercially available, for example, from EAS, Inc., Crystal Lake, Ill., and Johnson-Matthey, Malvern, Pa.
The U.S. EPA rule that was promulgated in March, 2004 requires CO removal efficiency to be at 58% or higher for two stroke, gas fueled engines. Preferably, the catalysts are selected sized to produce at least a 70% removal of CO and a 55% removal of formaldehyde. This will allow for a gradual degradation of catalyst efficiency over a sufficiently long period of time between periods of catalyst regeneration or replacement, preferably coinciding with other scheduled engine maintenance.
An example of a particularly preferred catalyst is provided by EAS, Inc. with the tradename ADCAT™ catalyst. This catalyst uses platinum on a stainless steel honeycomb substrate. After our experiments with this catalyst, a standardized size for the catalyst element was defined for use on all Ajax® engine models. Each Ajax® engine will use one of these catalyst elements per power cylinder. These elements are 12.5″ wide×34″ long×3.7″ thick. The face surface area and the thickness for the catalyst were determined from our tests and based on the flow area and an estimate of the exhaust residence time in the catalyst needed to produce the required emissions removal efficiencies.
The catalytic converter must provide the required emissions removal efficiencies throughout the normal engine operating range, which is 265 RPM to 440 RPM and from 50% to 100% torque. The above range extends from 60 to 200 BHP per power cylinder. The converter is required to operate properly with the wide range of fuel gases, which are typically used at various field sites. This variety includes fuels having lower heating values (LHV) from 450 to 1500 BTU/ft 3 . On the lower end of the LHV range, these fuels contain high quantities of inert gases like CO 2 and N 2 . On the upper end of the LHV range, these fuels contain high quantities of the heavier hydrocarbons, like propane, butane, and small amounts of pentane.
The primary areas of focus for our experiments were: (1) operation near the design rating, which is 200 BHP per cylinder, and (2) use of pipeline quality fuel gas, which consists mainly of methane and has an LHV of 950 BTU/ft 3 .
Catalyst Retaining Rack:
A catalyst element retaining rack is located inside the second chamber or volume of the silencer/catalytic converter unit (See FIGS. 3 and 6 ). This concept results in providing exhaust silencing while also serving as a catalyst housing. It also assures that the catalyst operating temperatures are high enough to achieve large removal efficiencies for the exhaust emissions.
Catalyst Surface Area and Residence Time:
Based on our testing to date, we expect that the engine will operate for more than 4000 hours before regeneration of the catalyst elements is needed. Measurement of CO before and after the catalyst is the preferred method for determining when the catalyst needs to be regenerated. At the end of our 500-hour lab test, the CO removal efficiency was about 92%. We expect that more than six months of continuous operation can be completed before the CO removal efficiency drops to the 58% level.
Preferably, there is one catalyst element per power cylinder of the engine. The catalyst element in one embodiment is 12.5″ wide×34″ long×3.7″ thick. Therefore, the overall width of a set of catalyst elements is equal to the number of power cylinders times the width of a single catalyst element, which in this case the width is 12.5″.
This catalyst element weighs 45 lbm. As a result, these catalyst elements can be installed without the crane and installation/removal device. However, in an earlier embodiment, a single round catalyst element was used for the lab tests and it weighed more than 200 lbm. This larger and heavier catalyst element required the use of a hoist and installation/removal device shown in FIG. 10 .
Based on our tests, we have determined a direct relationship between exhaust flow and catalyst surface area and between exhaust flow and catalyst thickness. If less catalyst is used, then the emissions removal efficiencies are inadequate. If more catalyst is used, then the removal efficiencies for CO, VOC's and H 2 CO are increased, but the NO X increase across the catalyst becomes unacceptable.
The total face surface area for the catalytic elements is preferably from about 20 to about 30 sq. in., more preferably from about 24 to about 28 sq. in., for each 100 actual ft 3 /min of exhaust flow, where “actual” means that the flow is referenced to the exhaust temperature at the catalyst. For the EAS catalyst tested, the preferred total face surface area for the catalytic elements is from about 24 to about 28 sq. in. for each 100 actual ft 3 /min of exhaust flow.
The effective residence time for exhaust to spend in the catalyst is preferably from about 0.025 to about 0.050 seconds, more preferably from about 0.030 to about 0.040 seconds, and yet more preferably from about 0.031 to about 0.037 seconds. For the EAS catalyst tested, the effective residence time was preferably from about 0.031 to about 0.037 seconds. The term “effective residence time” is based on the thickness of the catalyst element. Actual residence time would be slightly higher because the path traveled through the catalyst is slightly longer than a straight line.
Relative to the EAS catalyst tested, other catalysts can have the same or different amounts of noble metal and the same or different exposed areas of the catalyst material to the exhaust passing through the catalyst element, depending on their internal structure. The above preferred ranges for the EAS catalyst would be good initial estimates for other catalysts, but routine testing of the catalysts can be used to determine their optimum face surface area and residence time factors.
Catalyst Location:
The preferred location for the catalyst is determined from the following factors:
a. Exhaust Tuning:
The exhaust is tuned to maximize the power output from a two-stroke engine. This involves the length of the exhaust pipe from the power cylinder to the end of the exhaust pipe. As is known to those skilled in the art, the exhaust pipe length is dependent on the swept volume for the power cylinder, the crank angle at which the exhaust ports open, and the rated speed for the engine. The preferred exhaust pipe length for the Ajax 2801LE, 2802LE, 2803LE, & 2804LE engines is 15′-6″.
b. Volume of the First Chamber of the Silencer/Converter:
The volume of the first chamber or volume of the silencer/converter is a function of the swept volume of the power cylinders (engine displacement). The volume of the first chamber of the silencer/converter is preferably equal to the number of exhaust pipes connected to that chamber times the swept volume for one cylinder times about 18, which is large enough to contain the exhaust from about 17 to 19 revolutions of the engine. This is the preferable volume to damp out the exhaust pulsations without upsetting the tuning effects gained from the tuned exhaust pipe.
c. Temperature:
To achieve acceptable emissions removal efficiencies, the oxidation catalyst must be in a location where the exhaust temperature is about 600° F., or higher. Therefore, the silencer/converter of the present invention is designed and installed to position the catalyst relative to the engine exhaust port such that this temperature is achieved.
Baffle and Flow Pipes:
A system of internal baffles and pipes is arranged inside the silencer/converter so that the catalyst element is protected from masking or fouling from liquid or particulate carryover into the exhaust. This system also protects the catalyst from sudden high pressure excursions and pulsations in the exhaust system (see FIGS. 3 and 6 ).
The main design feature that is pertinent to achieving a satisfactory catalyst life is based on causing the changes to the direction and to the flow rate of the exhaust prior to entering the catalyst. This feature results in minimal carry-over of liquid droplets and particulates to the catalyst.
The prior art silencers do not include considerations of limiting the carry-over of liquid droplets and particulates and they do not include any provision for the installation of a catalyst.
The new silencer/converter designs of the present invention have many similarities with the prior art silencer design by necessity since both designs perform the exhaust silencing function. However, the silencer/converter of the present invention includes additional features, which are described herein, relating to the incorporation and protection of the oxidation catalyst.
A baffle and flow pipes must be place in the silencer/converter ahead of the catalyst to protect the catalyst from liquid and particulate carry-over from the exhaust pipes.
A sufficient distance between (1) the exits of the flow pipes from the first chamber or volume into the second chamber or volume and (2) the catalyst face is preferred to allow the exhaust flow to be distributed evenly across the face of the catalyst. For example, with a silencer/converter cross sectional flow area of 8-12 ft 2 and an exhaust flow of about 1400-1600 actual ft 3 /min per engine cylinder, this distance is preferably a minimum of about 1½ feet.
The volumes of the chambers in the silencer/converter are dependent on the swept volume of the power cylinders. The flow areas of the pipes between these chambers are dependent on the total exhaust flow rate. Relative to protecting the catalyst from masking due to liquid droplets or particulates, the main functions of the baffles and pipes are to:
1. Reduce the flow velocity as the exhaust enters the first volume chamber causing liquid and solid constituents to drop out of the exhaust stream. 2. Produce some radical changes in flow direction to promote the drop out process. 3. Increase the exhaust flow velocity as the exhaust passes through the pipes between the volume chambers. 4. Substantially reduce the amplitude of the exhaust pressure pulsations before the exhaust reaches the catalyst. 5. Provide an even distribution of exhaust flow across the face of the catalyst.
The exhaust velocity in the exhaust pipes at the point of entrance to the silencer/converter is 2900-3200 feet per minute at the design rated engine speed of 440 RPM with our standard production engines, which have a displacement volume of 2827 in 3 per cylinder. The exhaust velocity at the input face of the catalyst for the above conditions ranges from 500 to 600 feet per minute.
From the perspective of designing a successful oxidizing converter, the two important factors relating to chamber volumes are:
A first chamber volume that will damp out the exhaust pulsations, and
Enough length between the exits of the flow pipes to the second chamber to the catalyst face to allow the exhaust flow to be distributed evenly across the face of the catalyst. For example, with a silencer/converter cross sectional flow area of 8-12 ft2 and an exhaust flow of about 1400-1600 actual ft3/min per cylinder, this length would be a minimum of about 1½ feet.
The relationships of the other chamber volumes and flow areas between the chambers are important for exhaust noise silencing, but not for the catalyst application. These relationships are commonly used by manufacturers of exhaust silencers.
The silencer/converter system has been designed in both the vertical and horizontal configurations to cover the possible variations in field sites (See FIGS. 3 and 6 ).
Pressure Relief Valve:
A pressure relief valve (or valves) is (are) used to protect the catalyst elements from sudden high pressure excursions in the exhaust system (See FIGS. 3 and 6 ).
A pressure relief valve is preferably placed in the first volume chamber to protect the catalyst from high-pressure excursions in the exhaust system that are caused by occasional firing into the exhaust ports. Some incorrectly refer to these events as backfires.
Preferably, there is one relief valve per exhaust inlet or pair of exhaust inlets. The incoming exhaust is preferably aimed towards the pressure relief valve, which is generally located opposite from the exhaust inlets. The relief valve setting must accommodate the normal exhaust pressure fluctuations exhibited in the first volume chamber, but it must relieve immediately when a higher pressure pulse than normal occurs. The pressure relief valve needs to relieve at the lowest pressure that allows adequate safety margin from the normal engine operating conditions. By recording the exhaust pipe pressures as functions of time during normal operating conditions, the highest normal pressure pulse was determined to be about 3 psig. Allowing for about a one to two psi safety margin, the relief valve is set at 4-5 psig to protect the catalyst from a higher pressure excursion.
Lubricating Oil:
Unlike four stroke engines, two stroke engines must have lubricating oil added to the power cylinders. This oil is mixed with the fuel for gasoline engines and is directly injected into the power cylinders for natural gas fueled engines. Two stroke gas engine operation tends to form various deposits such as varnish, sludge and an ash residue that remains after the oil is burned during operation. Adding detergent/dispersant additives controls the varnish and sludge. However, these detergent/dispersant additives tend to leave a gray, fluffy ash residue after the oil has been burned. This ash residue is made up of metal sulfates from such additives as barium, calcium, phosphorus, zinc, magnesium and boron, which deactivate the exhaust catalyst by forming glassy-amorphous deposits, which prevent the exhaust gas from reaching the active surfaces of the catalyst.
The lubricating oil used in the present invention for the 2-stroke engine power cylinders is formulated to minimize the type of oil additives that would degrade the catalyst efficiency. The power cylinder lube oil is formulated so that the zinc content was reduced from about 300 ppm present in prior art oils to at most less than 10 ppm, preferably at most 5 ppm. Other metals that poison the catalyst are also preferably at low levels to avoid poisoning of the active sites of the catalyst.
Such lube oils are formulated to reduce the metallic additives while increasing some of the non-metallic additives to provide acceptable lubricating properties for the 2-stroke natural gas fueled engine. The lube oil provided for the experiments conducted herein was formulated by ExxonMobil, which modified its Mobil Pegasus Special 10W-40 with the special additives, which reduce the zinc content to less than 5 ppm while maintaining the required lubrication properties.
Preferably, the lube oils have a very low ash content. The term “ash” refers to a metal-containing compound wherein the metal can be zinc, sodium, potassium, magnesium, calcium, lithium, barium, and the like, as measured by ASTM D874. Ash can also contain sulfur in the form of sulfated ash. The term “very low ash content” refers to less than 0.10 wt % ash content in the lubricating oil composition. Very low ash lube oils reduce the sulfur oil combustion products, which poison the oxidation catalyst by masking the catalyst active sites.
Other lube oils for 2-stroke natural gas engines are commercially available, which have low metals content. Examples of these include Mysella 40 available from Shell Lubricants (0.01 sulfated ash % by mass, 0 zinc content % wt, 0.025 phosphorous % wt, 0 calcium % wt) and Chevron HDAX ashless gas engine oils (nil sulfated ash % wt, less than 10 ppm zinc content, 670 ppm phosphorous). As earlier noted, phosphorous and calcium also poison catalyst active sites.
If the lube oil were not reformulated to have a low zinc content and to have a very low ash content (according to ASTM method D874), then the initial emissions removal efficiencies for the catalyst would be about equal to the efficiencies measured during our experiments, but the catalyst would be poisoned and masked quicker. Since the emissions removal efficiencies would be expected to fall to unacceptable levels in less than six months of operation, the effects of operating without the reformulated oil were not measured. As noted earlier, metallic additives in the oil would cause catalyst degradation problems.
Catalyst Installation Rig (Optional Equipment):
An installation and removal rig for the catalyst element with the catalyst rack was designed so that a catalyst element and catalyst rack can be lifted, inserted into the converter housing, and extracted from the housing while working from the ground level (See FIG. 10 ). The rig has a tray with four lifting points. A heavy catalyst element with its catalyst rack is placed on the tray. Chains are attached to the lifting points. A hoist or block and tackle arrangement with a lifting cable or chain is attached to the chains attached to the tray. Once the tray is level with the access flange for the catalyst retainer rack housing and drawer slide in the second or catalyst chamber, the tray is secured to the access flange. Attached to tray opposite the access flange attachment is a rotatable wheel having female screw portion that receives an elongated male threaded rod that is attached on one end thereof to the catalyst rack at a point opposite to the access flange. The rotatable wheel is rotated using a sprocket and chain assembly or with a motor assist to push the catalyst rack in through the opening in the access flange onto the drawer slide or to withdraw the catalyst retainer rack from the second or catalyst chamber. Once the catalyst rack is fully inserted and resting on the drawer slide, the threaded rod is released from its attachment point on the catalyst rack and the access cover door is replaced on and attached to the access flange.
Materials of Construction:
Nearly all of the silencer/converter is constructed of 10-gauge sheet steel, but there are several places where an inner shell of the same material is used to produce the appropriate sound deadening qualities.
The frames for the catalyst elements and portions of the retaining rack for the elements are preferably fabricated with stainless steel.
The gaskets for the catalyst and for the access cover door are produced with a high temperature fiberglass material that provides good sealing up to about 900° F.
New or Retrofits:
This combination silencer/converter is preferably designed to be interchangeable with prior art exhaust silencers and can therefore be used on a new engine unit or as a field retrofit on an existing engine unit. In a retrofit situation, the engine lubricant would be changed to a lubricating engine oil having a zinc content less than 10 ppm, preferably less than 5 ppm, and is preferably also very low ash content. Such lubricating engine oils are used in conjunction with the silencer/converter unit of the present invention to extend the duration for achieving satisfactory emissions removal efficiencies for the catalyst.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic side elevation of a prior art internal combustion engine with a silencer.
FIG. 2 is a schematic side elevation of an embodiment of an internal combustion engine with a silencer/catalytic converter according to the present invention.
FIG. 3 is a schematic side elevation of a vertical embodiment of a silencer/catalytic converter according to the present invention.
FIG. 4 is a side view of the catalyst retainer rack of FIG. 3 with two catalyst elements.
FIG. 5 is a top view of a section of the catalyst chamber of FIG. 3 showing the catalyst retainer rack, its gasket, and the shoulder located within the catalyst chamber for seating the gasket.
FIG. 6 is a schematic side elevation and a partial cross-section of a horizontal embodiment of a silencer/catalytic converter according to the present invention.
FIG. 7 is a schematic end elevation of the silencer/catalytic converter in FIG. 6 showing the relative placement and angle of the exhaust inlet and the relief valve.
FIG. 8 is a side view of the catalyst retainer rack of FIG. 6 with four catalyst elements.
FIG. 9 is a top view of a section of the catalyst chamber of FIG. 6 showing the catalyst retainer rack, its gasket, and the shoulder located within the catalyst chamber for seating the gasket.
FIG. 10 is a schematic top view of an embodiment of an optional catalyst installation and removal system according to the present invention.
FIG. 11 is a graph of catalyst efficiency curves showing previous industry results using dashed lines and the results obtained during the experiment reported herein.
DETAILED DESCRIPTION
Referring to FIG. 1 , a prior art stationary two-stroke or two-cycle internal combustion engine system 500 is shown having from one to four cylinders, with only one cylinder 30 schematically shown. The cylinder 30 has an inlet port 36 and an exhaust port 38 . A gaseous hydrocarbon fuel is fed into each cylinder 30 at the appropriate point in the engine's cycle via line 32 in fluid communication with the inlet port 36 . A source of lubricating engine oil is provided to the engine via line 34 . Details of the engine have been omitted from FIG. 1 for the sake of clarity. Stationary natural gas fueled 2-stroke engines typically operate at constant speeds in the range of from 200 to 1000 rpm, more typically 250 to 500 rpm.
In operation, a piston reciprocates within each cylinder 30 of the stationary engine. As the piston descends within the cylinder moving away from the cylinder head, it opens an inlet port 36 , through which a gas or a mixture of gases is admitted and flows into the cylinder 30 . At this time, the cylinder 30 is filled with gases which are products of combustion. In certain designs of engine, a mixture of gaseous fuel and air is admitted into the cylinder 30 through the inlet port 36 at this time. In other designs of engine, such as the Ajax® engines referred to above, air alone is admitted to the cylinder 30 through the inlet port 36 . At the same time that the inlet port 36 is open, the descending piston also uncovers an exhaust port 38 , through which the burnt gases leave the cylinder 30 via exhaust pipe 40 , to form the exhaust gas of the engine. The action of the freshly charged gases entering the cylinder 30 through the inlet port 36 serves to assist with forcing the burnt gases out of the exhaust port 38 , referred to as scavenging. The exhaust gases travel through the exhaust pipe 40 , and then through the silencer 46 and exhaust stack 48 .
Referring now to FIG. 2 , there is shown an engine system 600 according to the present invention. System 600 requires the use of a stationary natural gas fueled 2-stroke engines that typically operate at constant speeds in the range of from 200 to 1000 rpm, more typically 250 to 500 rpm. These engines operate on a normally gaseous hydrocarbon as its fuel, for example, methane, ethane, propane and butane. System 600 differs from prior art system 500 in that the lubricating engine oil via line 34 is changed to be a lubricating engine oil via line 52 which has at most 10 ppm zinc and is preferably very low in ash content. Additionally, the silencer 46 and its exhaust stack 48 are changed to a silencer/catalyst converter unit 50 according to the present invention with its exhaust stack 54 to reduce the emissions in the exhaust. The silencer/converter unit 50 can be in vertical or horizontal embodiments. An example of a vertical embodiment is unit 100 and of a horizontal embodiment is unit 200 , which are discussed further below. Though not shown, in another embodiment, an exhaust manifold can also be used. For example, the exhaust pipe 40 is connected to the exhaust manifold 42 (instead of directly to the silencer/catalyst converter unit 50 ) and a silencer line 44 is connected on one end to the exhaust manifold 42 and on the other end to the silencer/catalyst converter unit 50 .
Referring now to FIG. 3 , there is shown a schematic side elevation of a vertical embodiment of a silencer/catalytic converter unit 100 according to the present invention. Unit 100 has an outer shell 101 with a lower head 132 and an upper head 133 enclosing a first volume chamber 134 , a second volume chamber 136 , and a third volume chamber 138 vertically positioned relative to each other. A first baffle 102 separates the first volume chamber 134 and the second volume chamber 136 . A second baffle 104 separates the second volume chamber 136 and the third volume chamber 138 . The second chamber 136 has a catalyst holding area 116 having a catalyst access door 118 .
Referring now to FIG. 4 , there is shown a side view of a section of a catalyst holding area 116 of the catalyst or second volume chamber 136 . The catalyst holding area 116 includes the catalyst retainer rack 128 that rides on the rack slide 129 , a gasket 130 for the catalyst rack 128 , and a shoulder 126 located within the catalyst chamber 136 for seating the gasket 130 . Any suitable means for seating the catalyst rack 128 against the shoulder 126 with the gasket 130 between them can be used, for example, a cam device (not shown). An access door 118 is used to access the catalyst rack 128 for removing or installing the catalyst elements 124 . A top view of the catalyst retainer rack 128 with two catalyst elements 124 is shown in FIG. 5 .
Referring again to FIG. 3 , the exhaust from the engine enters the first volume chamber 134 through exhaust inlet 110 . The number of exhaust inlets 110 depends on the number of cylinders in the engine, typically one for each cylinder or a pair of cylinders. A relief valve 114 is generally positioned opposite the exhaust inlet 110 . Due to the baffle 102 and changing the direction of flow of the exhaust within the first volume chamber 134 , liquid and solid particulates are at least partially removed from the exhaust. These collect in the lower silencer head 132 . A drain line and valve assembly 112 is attached to the bottom of the lower silencer head 132 to allow removal of any accumulated liquid and particulate solids.
The volume of the first volume chamber 134 is sufficient to dampen spurious pressure excursions or pulsations to avoid damage to the catalyst elements 124 . The exhaust then exits the first volume chamber 134 through flow pipes 106 into the second volume chamber 136 . The leading face of the catalyst elements 124 are spaced from the exit of the flow pipes 106 to allow a uniform flow of the exhaust across the face of the catalyst elements 124 to more fully utilize the available catalyst active sites in the catalyst elements 124 .
After the exhaust passes through the catalyst elements 124 , the exhaust exits the second volume chamber 136 into the third volume chamber 138 through flow pipes 108 . The exhaust then exits the third volume chamber 138 through flow pipe 120 , which enters the exhaust stack 122 .
The volume of the second volume chamber 136 and the volume of the third volume chamber 138 , along with the volume of the first volume chamber 134 , are to produce the silencing effects of the unit 100 .
Referring now to FIG. 6 , there is shown a schematic side elevation in partial cross-section of a horizontal embodiment of a silencer/catalytic converter unit 200 according to the present invention. Unit 200 has an outer shell 140 with a first outer head 142 and a second outer head 143 enclosing a first volume chamber 174 , a second volume chamber 175 , a third volume chamber 176 horizontally positioned relative to each other with the third volume chamber 176 between the first and second volume chambers 174 and 175 , respectively. A fourth volume 178 is located above the third volume chamber with a fifth volume chamber 179 above the fourth volume chamber. A first baffle 146 separates the first volume chamber 174 and the third volume chamber 176 . A second baffle 147 separates the second volume chamber 175 and the third volume chamber 176 . A third baffle 148 separates the third volume chamber 176 and the fourth volume chamber 178 . The fourth volume chamber 178 has a catalyst holding area 164 having a catalyst access door 165 . A fourth baffle 150 separates the fourth volume chamber 178 and the fifth volume chamber 179 .
Referring now to FIG. 8 , there is shown a side view of a section of a catalyst holding area 164 of the catalyst or fourth volume chamber 178 . The catalyst holding area 164 includes the catalyst retainer rack 168 that rides on the rack slide 169 , a gasket 170 for the catalyst rack 168 , and a shoulder 172 located within the catalyst chamber 178 for seating the gasket 170 . Any suitable means for seating the catalyst rack 168 against the shoulder 172 with the gasket 170 between them can be used, for example, a cam device (not shown). An access door 165 is used to access the catalyst rack 168 for removing or installing the catalyst elements 166 . A top view of the catalyst retainer rack 168 with four catalyst elements 166 is shown in FIG. 9 .
Referring again to FIG. 7 , the exhaust from the engine enters the first volume chamber 174 through exhaust inlets 158 A and 158 B. The exhaust from the engine also enters the second volume chamber 175 through exhaust inlets 158 C and 158 D. In this embodiment, the unit 200 is for a 4-cylinder engine. The number of exhaust inlets 158 depends on the number of cylinders in the engine, typically one for each cylinder or a pair of cylinders. In this embodiment, the engine has 4 cylinders and there are four exhaust inlets 158 A, 158 B, 158 C and 158 D. A relief valve 162 is generally positioned opposite the exhaust inlets 158 . In this embodiment, there are two relief valves 162 —one for each of the first volume chamber 174 and the second volume chamber 175 . Each relief valve 162 is positioned generally opposite from and between the respective exhaust inlets Therefore, one relief valve 162 is generally opposite and between the exhaust inlets 158 A and 158 B; and the other relief valve 162 is generally opposite and between the exhaust inlets 158 C and 158 D. When looking down the long axis L of the unit 200 , the angle A between the axis R of the relief valve 162 and the axis E of the exhaust inlet 158 is at most 45 degrees.
Due to the baffles 146 , 147 and 148 , plus changing the direction of flow of the exhaust within the first, second and third volume chambers 174 , 175 and 176 , liquid and solid particulates are at least partially removed from the exhaust. These collect in the bottom of chambers 174 , 175 and 176 . A drain line and valve assembly such as assembly 112 shown in FIG. 3 are added to the bottoms of each of chambers 174 , 175 and 176 to allow removal of any accumulated liquid and particulate solids therein.
The volumes of chambers 174 , 175 and 176 are sufficient to dampen spurious pressure excursions or pulsations to avoid damage to the catalyst elements 166 . The exhaust exits the first volume chamber 174 through flow pipes 152 into the third volume chamber 176 . The exhaust exits the second volume chamber 174 through flow pipes 153 into the third volume chamber 176 . The exhaust exits the third volume chamber 176 through flow pipes 154 into the catalyst chamber or fourth volume chamber 178 . The leading face of the catalyst elements 166 are spaced from the exit of the flow pipes 154 to allow a uniform flow of the exhaust across the face of the catalyst elements 166 to more fully utilize the available catalyst active sites in the catalyst elements 166 .
After the exhaust passes through the catalyst elements 166 , the exhaust exits the fourth volume chamber 178 into the fifth volume chamber 179 through flow pipes 156 . The exhaust then exits the fifth volume chamber 179 through the exhaust stack 160 , which optionally has a flange as shown herein for attaching to a stack extension (not shown).
The volume of the fourth volume chamber 178 and the volume of the fifth volume chamber 179 , along with the volume of chambers 174 , 175 and 176 , are to produce the silencing effects of the unit 200 .
Referring now to FIG. 10 , there is shown a top perspective elevation of an embodiment of a catalyst installation and removal system 300 according to the present invention used on a vertical unit 100 ′, which is similar to unit 100 , except that a single round catalyst element 124 ′ with a round catalyst rack 128 ′ is used instead. The system 300 was designed so that the catalyst element 124 ′ and catalyst rack 128 ′ can be lifted, inserted into the converter housing 302 , and extracted from the housing 302 while working from the ground level. The system 300 has a tray 304 with four lifting points 306 . A heavy catalyst element 124 ′ with its catalyst rack 128 ′ is placed on the tray 304 . Chains 308 are attached to the lifting points 306 . A hoist or block and tackle arrangement with a lifting cable or chain (not shown) is attached to a lifting eye 310 to which the chains 308 are attached. Once the tray 304 is level with the access flange 312 for the catalyst retainer rack housing 302 and drawer slide in the second or catalyst chamber, the tray 304 via its attachment ears 314 is secured to the access flange 312 . Attached to tray 304 opposite the access flange 312 attachment is a rotatable wheel 316 on a mount 317 , wherein the wheel 316 has a female screw portion that receives an elongated male threaded rod 318 that is attached on one end 320 to an attachment mount 322 on the catalyst rack 128 ′ at a point opposite to the access flange 312 . The rotatable wheel 316 is rotated using a sprocket and chain assembly or with a motor assist to push the catalyst rack 128 ′ in through the opening in the access flange 312 onto the drawer slide 129 (see FIG. 4 ) or to withdraw the catalyst retainer rack 128 ′ from the second or catalyst chamber 136 (see FIG. 3 ). Once the catalyst rack 128 ′ is fully inserted and resting on the drawer slide 129 , the threaded rod 318 is released from the attachment mount 322 on the catalyst rack 128 ′ and the access cover door 118 (see FIG. 3 ) is replaced on and attached to the access flange 312 .
Experiment:
A vertical silencer/catalytic converter unit according to the present invention was installed on an Ajax® DPC-2802LE engine in the Ajax R & D Lab, and was tested for nearly 500 hours with the engine operating at full speed, nearly full torque, and close to the full rated BHP.
The Ajax® DPC-2802LE engine is a two-stroke, lean burn, natural gas fired engine. It has 2 power cylinders, each with a bore of 15 inches and a stroke of 16 inches. The engine speed is 265 to 440 rpm. The prior art silencer was replaced with a vertical silencer/converter like that shown in FIG. 3 . However, the catalyst retaining rack was round as was the single catalyst element as shown in FIG. 10 . The catalyst was about 3½ feet in diameter, 3.7 inches thick and weighed about 200 lbm. The catalyst was ADCAT™ catalyst from EAS, Inc. This catalyst uses platinum on a stainless steel honeycomb substrate. A catalyst lifting rig as shown in FIG. 10 was used to lift and install or remove the catalyst and catalyst rack from the silencer/converter. The overall height of the silencer/converter unit without the exhaust stack was about 16 feet with a diameter of about 3½ feet. The volume of the first chamber 134 was about 72 cu. ft. The volume of the second chamber 136 was about 42 cu. ft. The volume of the third chamber 138 was about 31 cu. ft. The distance between the exit of the flow pipe 106 and the leading face of the catalyst element 116 was about 1½ feet. There were 2 exhaust inlet 110 from the exhaust pipe(s) connected to the exhaust ports of the engine. The conventional lubricating engine oil that the engine used had about 300 ppm zinc. This oil was replaced with a modified Mobil Pegasus Special 10W-40 formulated by ExxonMobil to have less than 5 ppm zinc and had an ash content of less than 0.1 wt %. The average exhaust temperature at the catalyst location in the silencer/converter was about 640 degrees F.
Initial performance for this invention achieved 93% removal of the CO emissions and 91% removal for the formaldehyde. Although these efficiencies were better than expected, a major feature of this invention is to prevent premature degradation of the catalyst removal efficiencies. As reported by DeFoort et al, their tests of oxidizing catalysts with 2SLB engines indicated that the removal efficiencies dropped to unacceptable levels within less than two weeks.
Catalyst efficiency curves are presented in FIG. 11 . These curves express the removal efficiencies vs. hours of operation for this invention as compared to those reported by DeFoort et al., who used oxidizing converters on 2SLB engines.
Standard exhaust emissions levels for Ajax® LE engines operating with pipeline quality fuel at the design rating with site elevations less than 1500 FASL (feet above sea level) are:
NOX=2.0 gm/BHP-hr CO=1.2 gm/BHP-hr NMHC=1.2 gm/BHP-hr H2CO=0.29 gm/BHP-hr
This catalyst and silencer/converter have been tested for nearly 500 hours at the design rating for the engine, and the oxidizing efficiencies were almost equal to the efficiencies recorded at the start of the tests.
Our Lab tests of the EAS oxidizing catalyst with the Ajax® DPC-2802LE engine included 430 hours with the full catalyst flow area, followed by 51 hours with 60% of the flow area. Our reasons for blocking 40% of the flow area were (1) to resolve the problem with NO X increase across the catalyst and (2) to determine the amount of catalyst needed for field applications.
The results from the Lab tests are in the following Table, which includes five columns expressing the average engine data and catalyst data during five time periods of the testing, which are defined in the accumulated hours row of the spreadsheet.
The main conclusions from this testing are:
1. The CO and H2CO removal efficiencies are substantially maintained over these 500 hours. 2. Degradation of the removal efficiencies was minimal during the 481 hours of testing. These efficiencies dropped by only 2-3% during this phase of the test project. 3. The NOX increase across the catalyst was unacceptable during the first 430 hours of testing. This increase averaged 23% during this time. The source for the nitrogen that was being converted to NOX was the nitrogen containing compounds in the lube oil. Mobil reports that it is not viable to reduce these compounds by a significant amount. 4. With 40% of the catalyst flow area blocked off, the NOX increase is acceptable. During the last 30 hours of testing, this increase averaged less than 5%. Blocking 40% of the catalyst flow area had minimal effects on the removal efficiencies for the CO and H2CO. 5. Though emissions removal efficiencies are expected to degrade over time, removal efficiencies which should be achievable for at least six months are expected to be:
CO-70% reduction H2CO-60% reduction.
TABLE
Average Data
During 481 Hours of Catalyst Operation
Catalyst Type & Flow Area
EAS—100%
EAS—100%
EAS—100%
EAS—60%
EAS—60%
Hours Accumulated with Catalyst
0-60
60-231
231-430
430-451
451-481
Engine Speed
440
440
440
440
440
BHP
361
352
352
352
384
(% of Full Rated BHP)
(94%)
(92%)
(92%)
(92%)
(100%)
Exhaust Flow (SCFM)
1670
1670
1660
1650
1650
Exhaust Temp.
648
645
640
650
670
(° F. before catalyst)
Exhaust Temp.
608
608
600
612
636
(° F. after catatalyst)
% Oxygen in the Exhaust
14.2
14.3
14.2
14.3
13.8
Exhaust Press. at Silencer/
3.3
3.2
3.2
3.2
3.65
Converter Inlet (″H 2 O)
Pressure Drop across the Catalyst
0.4
0.5
0.5
0.55
0.9
(″H 2 O)
CO (gm/BHP-hr Before Catalyst)
1.4
1.4
1.3
1.4
1.7
CO (gm/BHP-hr After Catalyst)
0.07
0.10
0.09
0.11
0.14
CO (ppm Before Catalyst)
153
152
143
150
187
CO (ppm After Catalyst)
8
10
11
12
16
CO Removal Efficiency (%)
94.7
93.4
92.3
92.0
91.4
H 2 CO (gm/BHP-hr Before
0.16
0.16
0.19
0.15
0.18
Catalyst)
H 2 CO (gm/BHP-hr After Catalyst)
0.015
0.016
0.019
0.015
0.020
H 2 CO (ppm Before Cat.)
23
23
27
20
25
H 2 CO (ppm After Cat.)
2
2.3
2.9
2.0
2.7
H 2 CO Removal Efficiency (%)
91.3
90.0
89.3
90.0
89.2
NO x (gm/BHP-hr Before Catalyst)
1.04
0.85
0.9
0.70
1.80
NO x (gm/BHP-hr After Catalyst)
1.35
1.02
1.10
0.77
1.89
NO x (ppm Before Cat.)
70
56
60
47
123
NO x (ppm After Catalyst)
91
67
73
52
129
NO x Increase Across Catalyst (%)
30.0
19.6
21.7
10.6
4.9
While the preferred embodiments of the present invention have been shown in the accompanying figures and described above, it is not intended that these be taken to limit the scope of the present invention and modifications thereof can be made by one skilled in the art without departing from the spirit of the present invention. | A low emissions 2-stroke natural gas fueled engine includes at least one cylinder with an exhaust port in communication with a silencer/catalytic converter unit. The unit has first and second volumes in communication with each other. The first volume dampens spurious exhaust pressure excursions and removes particulates in the exhaust. The second volume houses an oxidation catalyst for treating exhaust to reduce exhaust emissions. The engine oil has at most 10 ppm zinc content to reduce metal poisons contained in the exhaust prior to contact with the oxidation catalyst. The engine oil preferably has a very low ash content to minimize sulfur combustion components in the exhaust to reduce masking of the oxidation catalyst. The first volume preferably has a pressure relief valve set to relieve at a pressure greater than the maximum normal operating pressure of the engine to avoid excessive pressure excursions of the engine exhaust from damaging the oxidation catalyst. | 5 |
RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Patent Application No. 62/045,489, filed Sep. 3, 2014, entitled “PARTITION DOOR HAVING SOUND ATTENUATING COATING” which is hereby incorporated by reference in its entirety, including, but not limited to, those portions that specifically appear hereinafter, this incorporation by reference being made with the following exception: In the event that any portion of the above referenced application is inconsistent with this application, this application supercedes said above referenced application.
BACKGROUND
[0002] 1. The Field of the Present Disclosure
[0003] The present disclosure relates generally to partition doors and sliding doors used to divide areas of a room or space, or to seal off a particular area. The partition doors may also include sound attenuating characteristics.
[0004] 2. Description of Related Art
[0005] A partition, accordion, or sliding door is generally used to divide areas of a room or space, or to seal off a particular area in case of needed security or possible danger. Partition doors are generally opaque, thus providing privacy between areas divided by the door. In addition to visual privacy, partition doors can provide a level of sound attenuation.
[0006] Sound attenuation in partition doors is often facilitated by the use of fiberglass insulation attached to an interior of the door. However, fiberglass insulation can be difficult to secure or fasten to the door, resulting in displacement of the insulation during use, which can require additional maintenance and replacement of the fiberglass insulation.
[0007] The features and advantages of the present disclosure will be set forth in the description which follows, and in part will be apparent from the description, or may be learned by the practice of the present disclosure without undue experimentation. The features and advantages of the present disclosure may be realized and obtained by means of the instruments and combinations particularly pointed out herein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008] The features and advantages of the disclosure will become apparent from a consideration of the subsequent detailed description presented in connection with the accompanying drawings in which:
[0009] FIG. 1 is a perspective view of a partition door;
[0010] FIG. 2 a is a bottom view of an embodiment of the present disclosure, including a slat and sound attenuating coating;
[0011] FIG. 2 b is a bottom perspective view of the embodiment of FIG. 2 a , including a slat and sound attenuating coating;
[0012] FIG. 2 c is a bottom perspective view of the embodiment of FIG. 2 a , including multiple slats configured in a collapsed position;
[0013] FIG. 2 d is a bottom perspective view of the embodiment of FIG. 2 a , including multiple slats configured in a partially opened position;
[0014] FIG. 3 a is a perspective view of the embodiment of FIG. 2 a , including a plurality of adjoined slats having a sound attenuating coating;
[0015] FIG. 3 b is a perspective view of the embodiment of FIG. 2 a , including a plurality of adjoined slats having a sound attenuating coating in an opened position;
[0016] FIG. 3 c is a bottom view of the embodiment of FIG. 2 a , including a plurality of adjoined slats having a sound attenuating coating;
[0017] FIG. 3 d is a side view of the embodiment of FIG. 2 a , including a plurality of adjoined slats having a sound attenuating coating;
[0018] FIG. 4 a is a side view of the embodiment of FIG. 2 a , including a slat having a sound attenuating coating;
[0019] FIG. 4 b is a side view of a bottom portion the embodiment of FIG. 2 a , including a slat having a sound attenuating coating;
[0020] FIG. 4 c is a side view of the embodiment of FIG. 2 a , including a hinge coupled to a slat having a sound attenuating coating;
[0021] FIG. 4 d is a bottom view of the embodiment of FIG. 2 a , including a slat having a sound attenuating coating;
[0022] FIG. 5 is a schematic view of a process for applying a sound attenuating coating to a partition door slat;
[0023] FIG. 6 is a transmission loss chart for a sample door having fiberglass insulation;
[0024] FIG. 7 is a transmission loss chart for a sample door having a single layer of sound attenuating coating; and
[0025] FIG. 8 is a transmission loss chart for a sample door having a double layer of sound attenuating coating.
DETAILED DESCRIPTION
[0026] For the purposes of promoting an understanding of the principles in accordance with the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the disclosure is thereby intended. Any alterations and further modifications of the inventive features illustrated herein, and any additional applications of the principles of the disclosure as illustrated herein, which would normally occur to one skilled in the relevant art and having possession of this disclosure, are to be considered within the scope of the disclosure claimed.
[0027] It must be noted that, as used in this specification and the appended claims, the singular forms “a,” “an,” and “the” include plural referents unless the context clearly dictates otherwise.
[0028] In describing and claiming the present disclosure, the following terminology will be used in accordance with the definitions set out below.
[0029] As used herein, the terms “comprising,” “including,” “containing,” “characterized by,” and grammatical equivalents thereof are inclusive or open-ended terms that do not exclude additional, unrecited elements or method steps.
[0030] Applicant has discovered a novel partition door having a sound attenuating coating, eliminating a need for additional or alternative sound attenuating material, and a method or process for applying the sound attenuating coating to an interior surface of a partition door.
[0031] FIG. 1 illustrates an exemplary embodiment of a partition door 100 . The partition door 100 includes a plurality of adjoined slats 102 . Each slat 102 is suspended from a track 104 such that each of the slats 102 hangs vertically from the track 102 toward a floor 106 , partitioning a room or other desired space. Each of the slats 102 are hinged or coupled to an immediately adjacent slat 102 via a hinge 108 . The hinges 108 can be made of a malleable or flexible material that enables the slats 102 to bend with respect to adjacent slats 102 , in an accordion-type fashion, while also maintaining a connection between the slats 102 .
[0032] A set of adjoined and adjacent slats 102 form a wall. The partition door 100 includes two walls (only one wall is illustrated in FIG. 1 ) substantially abutting one another along a vertical axis of each wall. Thus, each wall includes an exterior surface and an interior surface. The interior surface substantially abutting the opposing wall.
[0033] Each of the slats 102 can be made of metal, such as aluminum, or wood, polymer or other desired rigid or semi-rigid material. The slats 102 can be substantially planar or can have a waved shape as shown in FIGS. 2 a - 4 d . The slats 102 can be approximately 4 inches in width, for example, and have a height that corresponds to the height of a room or desired space to ensure substantially complete partitioning of the desired room or space. The slat 102 widths may also be approximately 4.5 inches, or any other desired width.
[0034] FIGS. 2 a - d , 3 a - d , and 4 a - d show a series of adjoined slats 102 that include a sound attenuating coating 110 . The sound attenuating coating 110 can be applied and fixed to an inner surface of the slats 102 . As shown in FIGS. 2 a - 4 d , 3 a - d , and 4 a - d , the coating 110 can be applied and fixed to the center (or any other desired portion of the slat 102 , or over the entire inner surface of the slat 102 ) of the slat 102 , along a vertical axis of the slat 102 , such that the coating will cover approximately 4 inches of the width of the slat 102 and extend substantially the entire vertical height (or length) of the slat 102 . Alternatively, the coating 110 can cover the entire inner surface of the slat 102 or a smaller desired surface area of the slat 102 .
[0035] The coating 110 acts as a sound barrier and reduces the sound transfer between areas that are partitioned by the door 100 . The coating 110 can replace more traditional insulators, like fiberglass, which can be more difficult to install and attach to the slats 102 , and usually requires insulation fastening elements to attach the insulation to the slats 102 .
[0036] Additionally, traditional insulators often need frequent maintenance due to a tendency for the traditional insulators, particularly fiberglass, to be displaced from the corresponding slats 102 or otherwise become damaged during use of the door. The displacement of the fiberglass insulation can cause the fiberglass to break apart and release airborne particulate into the surrounding air. Airborne fiberglass particles can become a significant health concern to nearby people or animals, for example, causing respiratory problems. Traditional insulators also tend to have lower sound attenuating capabilities at lower frequencies, however, the coating 110 out performs traditional insulators, specifically fiberglass insulation, in attenuating low frequency sound.
[0037] In contrast, the coating 110 adheres directly to the surface of the slats 102 and therefore remains fixed to the slat 102 for substantially the life of the door 100 , thereby eliminating any airborne fiberglass particles that can be problematic with the use of traditional insulation. The coating 110 is also more efficiently fixed to the slats 102 , when compared to fixing traditional insulators to the slats 102 , through a spray application process described in more below and illustrated in FIG. 5 . The spray application process saves time and installation cost because the spray application process can be performed as part of the manufacturing process of the slats 102 . Therefore, there is no need to add insulation on site or during the door 100 installation process.
[0038] The coating 110 also increases the weight of the door 100 , when compared to traditional fiberglass insulation. The added weight aids in reducing swaying of the door 100 during use, thereby improving the sliding of the door 100 and reducing potential damage caused by frequent or excessive sway of door 100 during operation. The added weight and uniform distribution of the coating 110 also act to reinforce the slats 102 , providing additional strength and durability to withstand minor impacts during use and operation of the door 100 .
[0039] It is estimated that use of the coating 110 may increase the lifetime and longevity of the door 100 by approximately 85% over the traditional use of fiberglass insulation with conventional attachment features. Additionally, the use of the coating 110 may even increase the lifetime and longevity of the door 100 by 20% over alternative fiberglass insulation configurations having improved mechanical attachment features. Furthermore, due to the added weight, strength, and stabilizing characteristics of the coating 110 , the door 100 may more effectively absorb and evenly distribute impact energy, which can significantly reduce damage to the door caused by impacts or other unintended manipulation of the door, which might otherwise cause damage.
[0040] The uniform distribution and relatively small thickness of the coating 110 , when compared to fiberglass insulation, also enable the door 100 to more completely compress adjacent slats 102 when the door 100 is in an open position (like a closed accordion), increasing the space efficiency of the door 100 .
[0041] FIG. 6 provides a transmission loss chart which includes the transmission loss of a sample door having fiberglass insulation. As shown in the chart, the fiberglass qualifies as a Sound Transmission Class (STC) 38 and an Outside Inside Transmission Class (OITC) 25 . ASTM publications E413-10 “Classification for Rating Sound Insulation” and E1332-10a “Standard Classification for Rating Outdoor-Indoor Sound Attenuation” are now incorporated herein in their entireties by this reference.
[0042] FIG. 7 provides a transmission loss chart that includes the transmission loss of a sample door having a single layer of the coating 110 , having a total thickness of approximately 0.09 inches. As shown on the chart, the single layer of coating 110 qualifies as a STC 39 and an OITC 28.
[0043] FIG. 8 provides a transmission loss chart that includes the transmission loss of a sample door having two layers of the coating 110 , having a total thickness of approximately 0.18 inches. As shown on the chart, the double layer of the coating 110 qualifies as a STC 42 and an OITC 30.
[0044] Comparing the test results shown in the transmission loss charts in FIGS. 6-8 , the coating 110 significantly improves the sound attenuating capabilities of the sample door. Some of the most significant sound attenuation improvements between the coating 110 and the fiberglass insulation occur at the lower frequency range (50-800 Hz), which can greatly improve the performance of the door 100 . For example, fiberglass has a transmission loss of 11 dB at 50 Hz, however, a single layer of coating offers a transmission loss of 13 dB at 50 Hz and a double layer of the coating 110 offers a transmission loss of 14 dB at 50 Hz. In another example, the fiberglass has a sound transmission loss of 20 dB at 160 Hz, however a single layer of the coating 110 offers a transmission loss of 23 dB at 160 Hz and a double layer of the coating 110 offers a transmission loss of 28 dB at 160 Hz.
[0045] The coating 110 can be a polyurea material that is designed to be applied to and permanently fixed directly to the slats 102 . The coating has adhesive characteristics which enable it to adhere directly to the slat 102 without the need for additional adhesives or a mechanical fixation element. The coating 110 can be designed with an extended gel time for better leveling, forming a substantially planar interior surface, and high abrasion resistance for demanding industrial applications. The coating 110 can also provide less shrinkage and improved elongation, thus providing for efficient and reliable containment on the inner surface of the slats 102 . The coating 110 is also designed to provide a continuous, seamless membrane over the surface of the slats 102 .
[0046] The coating 110 can include, for example, the following composition and ingredients: dialkylaminodiphenylmethane at 10-30% by weight, 2,4-diethyltoluenediamine at 7-13% by weight, triethanolamine at 5-10% by weight, poly(oxy(methyl-1,2-ethanediyl)), aplpha-(2-aminomethylethyl) omega-(2-aminomethylethoxy) at 5-10% by weight, and 2,6-diethyltoluenediamine at 1-5% by weight. Other polyurea and polymer materials having similar sound attenuating characteristics can also be used to compose the coating 110 .
[0047] The coating 110 can also be characterized by its performance properties, namely, an ultimate elongation of approximately 370% and a tensile strength of approximately 2000 PSI, a tear strength of approximately 365 PLI, a hardness of approximately 45 Shore D and a dielectric strength of approximately 433V/mil. The coating 110 can also be water resistant and provide protection against corrosion.
[0048] As shown in FIG. 5 , the coating 110 can be applied to a corresponding slat 102 as part of the manufacturing process, as opposed to on site as part of the door 100 installation process. The slat 102 is formed to the desired specification in a conventional process using a roll form mechanism 112 . Upon exiting the roll form mechanism 112 , the slat 102 can be forced along a conveyor ramp 114 .
[0049] Before the coating 110 can be applied to the slat 102 , the slat 102 can pass through a cleaning station 116 where the surface of the slat 102 is cleaned of dirt, soluble salts, dust, oils, grease, chalking and contaminants. The cleaning station 116 can include a vacuum, blow-off, solvent cleaning, and/or water-wash containing salt solubilizing agents.
[0050] After passing through the cleaning station 116 , the slat 102 then passes through a first spray application station 118 where a first layer of the coating 110 is sprayed onto the surface of the slat 102 . As described above, the coating 110 is applied along the entire length of the slat 102 and over a desired width, for example, 4 inches of a 4.5 inch slat 102 , although alternative widths and configurations can be used. The thickness of the coating 110 can usually be between 60-200 mils.
[0051] To further improve the sound attenuation of the coating 110 , a second layer of the same sound attenuating coating can be applied over the top of the first layer of the coating 110 , with each layer having a thickness between 60-100 mils. Thus, after the slat 102 has passed through the first spray application station 118 the coating thickness may be increased by a second layer of the coating 110 which can be applied in the same or similar manner.
[0052] After passing through the first spray application station 118 , the slat 102 will continue along the conveyor ramp 114 through a dryer 120 . The dryer 120 can be an air dryer, possibly blowing heated air, to speed the drying and curing of the first layer of the coating 110 .
[0053] After passing through the dryer 120 , the slat 102 can then pass through a second spray application station 122 where a second layer of the coating 110 can be sprayed onto the surface of the slat 102 , if a second layer is desired. There may be circumstances where one, single layer of the coating 110 is sufficient and/or desirable. As with the first layer, the second layer of the coating 110 is applied along the entire length of the slat 102 and over a desired width, for example, 4 inches of a 4.5 inch slat 102 . The total thickness of the coating 110 after passing through the second spray application station 122 can usually be between about 60 and about 200 mils.
[0054] After passing through the second spray application station 122 the slat 102 can be sheared, or otherwise cut, to the desired length and set aside to fully cure. Drying and curing times of the coating 110 include: 10-15 seconds to gel, 20-30 seconds until tack free, approximately 8 hours until a hard dry, and can be immersed in water, without detrimental effect, in approximately 24 hours.
[0055] The process of coating the slats 102 can be continuously performed until the desired number of slats has been reached. After curing of the coating 110 is complete, the slats 102 can be transported to a desired site to be assembled as part of the partition door 100 .
[0056] It is to be understood that the above-described arrangements are only illustrative of the application of the principles of the present disclosure. Numerous modifications and alternative arrangements may be devised by those skilled in the art without departing from the spirit and scope of the present disclosure are intended to cover such modifications and arrangements. Thus, while the present disclosure has been shown in the drawings and described above with particularity and detail, it will be apparent to those of ordinary skill in the art that numerous modifications, including, but not limited to, variations in size, materials, shape, form, function and manner of operation, assembly and use may be made without departing from the principles and concepts set forth herein. | A partition door including, a plurality of door slats, wherein each of the door slats are suspended from a track and extend vertically toward a floor. Each of the door slats are moveable in a generally horizontal direction. The partition door also includes a plurality of hinges, each hinge coupling adjacent door slats. The partition door further including a sound attenuating coating fixed to a first surface of at least one of the plurality of door slats. | 4 |
BACKGROUND OF THE INVENTION
The present invention relates to a thermal transfer printing apparatus, and, more particularly, to a thermal transfer printing apparatus in which a pixel is formed by a plurality of dots in a matrix form, and can be printed in a halftone mode, or with gradation or gray levels.
In a thermal transfer printing apparatus, a thermal head (printing head) is urged against printing paper through an ink film (normally having a ribbon-shape), and an ink on the ink film is melted by heat generated when heating resistors constituting the thermal head are energized. Thus, the melted ink is transferred to the printing paper so as to form a dot image corresponding to the energized resistors. In this apparatus, each dot can only be binary-controlled as to whether or not the ink is transferred. Therefore, in order to print a halftone image such as a picture, a so-called binary area modulation method is generally adopted. In this method, a pixel must correspond to a plurality of dots in a matrix form. The number of dots which are energized and subjected to ink transferring, however, changes in accordance with the density of a pixel. A DITHER method, a micro-font method or the like are well known as binary area modulation methods.
However, the number of levels able to be represented by this area modulation method is limited. When a pixel has an n×n dot matrix configuration, the number of levels expressed is n 2 +1, including 0 level (the level of the printing paper). For example, in the case of a 4×4 dot matrix, 17 levels are provided. In general, a color image requires a resolution of 4 dots/mm or higher, and each color component requires 64 gray levels or more. In order to satisfy these requirements with the above-mentioned area modulation method, a pixel must be configurated by an 8×8 dot matrix, and a thermal head having a resolution of 32 dots/mm or higher is needed. Although a thermal head having a resolution of 16 dots/mm has been developed, it is difficult to realize one having a resolution of 32 dots/mm or higher. For this reason, in this area modulation method, requirements for the number of gray levels and resolution cannot be satisfied, and it is impossible to perform halftone printing having a gradation that in both smooth and fine.
In a thermal transfer printing apparatus, a portion designated to remain white in a high or medium density region may be colored due to heat pile-up of the thermal head. In contrast to this, an ink may not be transferred due to an insufficient amount of heat in a low density region. For this reason, a halftone image cannot be printed precisely.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a thermal transfer printing apparatus capable of printing a halftone image without degrading resolution.
According to the present invention, there is provided a thermal transfer printing apparatus comprising:
a thermal head comprised of a plurality of heating members aligned in line, each of the heating members transferring an ink to printing paper upon being heated so as to form one dot, the thermal head moving relative to the printing paper and defining a pixel using m×n heating members (m, n: positive integers); and
driving means connected to the thermal head, receiving an image signal indicating a multilevel density of each pixel, and heating a predetermined heating member of the m×n heating members defining each pixel, in accordance with a density of each pixel, so as to transfer the ink to the printing paper, thereby forming a dot having a size corresponding to the density of each pixel.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram showing a thermal transfer printing apparatus according to a first embodiment of the present invention;
FIGS. 2A to 2C are views showing the relationship between energy supplied to a printing head and the shape of a pixel formed to explain a principle of the first embodiment;
FIG. 3 is a graph showing the relationship between the energy supplied to the printing head in the first embodiment and an optical density of the pixel formed;
FIGS. 4A to 4C are views showing multilevel dot patterns, in respective density ranges, used for driving a printing head in a second embodiment;
FIG. 5 is a graph showing the relationship between energy supplied an an optical density of a pixel formed when the printing head is driven in accordance with the multilevel dot patterns shown in FIGS. 4A to 4C;
FIG. 6 is a table showing the relationship between the energy supplied to the printing head in the second embodiment and the halftone gradation level of the pixel formed;
FIG. 7 is a block diagram showing a multilevel dot pattern generator shown in detail in FIG. 1;
FIGS. 8A to 8H are timing charts showing an operation of the multilevel dot pattern generator shown in FIG. 7;
FIG. 9 is a block diagram showing a thermal head driver shown in FIG. 1;
FIGS. 10A to 10G are timing charts showing an operation of the thermal head driver shown in FIG. 9;
FIG. 11 is a graph showing the relationship between energy supplied to a thermal head and a temperature thereof;
FIG. 12 is a block diagram showing a thermal head shown in detail in FIG. 1;
FIGS. 13A and 13B are signal waveform charts showing an energy amount supplied to a head when the thermal head is at a normal temperature;
FIGS. 14A and 14B are signal waveform charts indicating that energy supplied to the thermal head at a high temperature can be decreased by decreasing a pulse width to compare with that at a normal temperature;
FIGS. 15A and 15B are signal waveform charts indicating that energy supplied to the thermal head at a high temperature can be decreased by decreasing an amplitude of a signal to compare with that at a normal temperature;
FIGS. 16A to 16C are views showing the effectiveness of a dot pattern used in a third embodiment;
FIGS. 17A to 17F are views showing a dot pattern used in the third embodiment and the shape of a pixel formed thereby;
FIGS. 18A and 18B are views showing a pattern and the shape of continuous pixels when a plurality of dot patterns used in the third embodiment are continuously arranged;
FIGS. 19A to 19N are views showing examples of dot patterns used in the third embodiment;
FIG. 20 is a view showing a dot pattern of the third embodiment when a pixel has a 2×2 matrix size;
FIG. 21 is a table showing the relationship between energy supplied to a printing head used in the third embodiment and a halftone gradation level of the pixel formed;
FIG. 22 is a graph showing the relationship between energy supplied and an optical density of a pixel formed when the printing head is driven using the multilevel dot pattern of the third embodiment;
FIGS. 23A to 23D are views showing dot patterns compared to indicate the effectiveness of a fourth embodiment;
FIGS. 24A to 24D views showing multilevel dot patterns, in respective density ranges, used for driving a printing head in the fourth embodiment;
FIGS. 25A and 25B are views showing a pattern when a plurality of dot patterns are continuously arranged in comparison with a conventional dot pattern;
FIGS. 26A and 26B are views showing the shape of a pixel formed when the thermal head is driven using the patterns shown in FIGS. 25A and 25B;
FIGS. 27A to 27D are views showing another example of multilevel dot patterns, in respective density ranges, used for driving the printing head in the fourth embodiment;
FIGS. 28A to 28D are views showing still another example of multilevel dot patterns, in respective density ranges, used for driving the printing head in the fourth embodiment;
FIGS. 29A to 29D are views showing still another example of multilevel dot patterns, in respective density ranges, used for driving the printing head in the fourth embodiment;
FIG. 30 is a view showing multilevel dot patterns used for driving a printing head in a fifth embodiment;
FIG. 31 is a view showing the shape of a pixel formed by driving the thermal head using the dot patterns shown in FIG. 30;
FIG. 32 is a view showing multilevel dot patterns compared to indicate the effectiveness of the fifth embodiment;
FIG. 33 is a view showing the shape of a pixel formed by driving the thermal head using the dot patterns shown in FIG. 32;
FIG. 34 is a view showing another example of multilevel dot patterns, in respective density ranges, used for driving the printing head in the fifth embodiment;
FIG. 35 is a view showing still another example of multilevel dot patterns, in respective density ranges, used for driving the printing head in the fifth embodiment;
FIG. 36 is a graph showing characteristics of multilevel dot patterns, in respective density ranges, used for driving a printing head in a sixth embodiment;
FIG. 37 is a block diagram showing an arrangement of the sixth embodiment;
FIG. 38 is a block diagram showing a dot pattern changing controller of the sixth embodiment;
FIG. 39 is a view showing dot patterns when a pixel has a 2×3 dot matrix size;
FIG. 40 is a view showing dot patterns when a pixel has a 3×4 dot matrix size; and
FIG. 41 is a view showing dot patterns when a pixel has a 4×2 dot matrix size.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A thermal transfer printing apparatus according to an embodiment of the present invention will be described with reference to the accompanying drawings.
A principle of the present invention will first be described. As described above, in a thermal transfer printing apparatus, a pixel corresponds to m×n dots in a matrix form (a dot is the minimum unit of a heating member constituting a printing head and capable of transferring an ink). The density of each pixel corresponds to the total amount of ink transferred in a matrix dot region corresponding to each pixel. Only when the amount of heat from a head exceeds a certain threshold level is an ink transferred to paper; otherwise, no transfer is performed. Conventionally, energy supplied to a head is a constant value higher than the threshold level, and the amount of ink transferred per dot is constant, through control, irrespective of the heat pile-up of the head. However, the present invention is based on the fact that the degree of heat of each heating member is proportional to the area of the dot formed. Thus, a specific dot is selected irrespective of density, and energy supplied to the selected specific dot is changed in accordance with density so as to control the degree of heat generated by this dot, thereby changing the total amount of ink transferred per pixel in accordance with the density.
FIG. 1 is a block diagram showing an arrangement of a thermal transfer printing apparatus according to a first embodiment of the present invention. An output from a graduation signal source 10 such as a memory is supplied to a multilevel dot pattern generator 12. Note that a gradation signal indicates the gray level of each pixel. The generator 12 generates a predetermined dot pattern for each pixel. Note that a pixel has an m x n dot matrix configuration, and a multilevel dot pattern constituted by specific dots therein is generated. That is, heating members corresponding to dots in this dot pattern are energized, the energization level (energy supply level) of each dot being controlled by the gradation signal. The thermal head 16 melts an ink while pressing printing paper 22 against the platen roller 18 through an ink ribbon 20, thereby transferring the ink onto the paper 22. A timing controller 24 for controlling various timings is connected to the gradation signal source 10, the multilevel dot pattern generator 12 and a driver circuit 14.
The operation of the first embodiment will be described. Note that, for the sake of simplicity, the generator 12 constitutes a pixel of a 3×3 dot matrix configuration, and generates a discrete dot pattern ("discrete" will be used as well as "single" hereinafter) of one dot at a central portion thereof. Energy supplied to each heating member is proportional to the amount of ink transferred to the printing paper. When a heating member of the head is energized at a low level, i.e., in the case of a low density level, a dot having a size corresponding to the heating member is formed on the printing paper, as shown in FIG. 2A. When the heating member of the head is energized at a medium level, i.e., in the case of a medium density level, a dot slightly larger than the size of the heating member is formed on the printing paper, as shown in FIG. 2B. When the heating member of the head is energized at a high level, i.e., in the case of a high density level, a dot considerably larger than the size of the heating member is formed on the printing paper, as shown in FIG. 2C.
For this reason, the energy supply level of the heating member and the optical density of a pixel can be controlled as shown in FIG. 3. When the energy supply level is smaller and lower than the threshold energy level required for the optimal transfer of ink, it is uncertain whether or not ink transfer has been performed. Therefore, since the optical density is also uncertain, a characteristic curve is indicated by a broken line.
According to the first embodiment, the energization level of the thermal head is determined in accordance with the gradation signal, and, as a result, a proper amount of ink corresponding to the density is transferred to the printing paper, thus printing each pixel in a halftone mode.
Note that in the first embodiment, only a discrete dot in 3×3 dots is used so as to provide halftone printing in accordance with a change in the energy supply level of the specific dot. However, a density may not satisfactorily be controlled by only the change in the energy supply level of the specific dot, and an embodiment solving this problem will be described hereinafter.
In a second embodiment in which the above problem is solved, the total optical density range is divided into three ranges, with specific dot patterns being assigned to respective density ranges. A block diagram of the second embodiment is substantially the same as that of the first embodiment shown in FIG. 1, except that the generator 12 constitutes a pixel of a 3×3 dot matrix, and generates a dot pattern (discrete dot pattern) constituted of one dot at an upper left corner, as shown in FIG. 4A, in a low density range; a dot pattern (stripe pattern) constituted by three dots included in a leftmost column, as shown in FIG. 4B, in a medium density range; and a dot pattern (L-shaped dot pattern) constituted by five L-shaped dots included, in a high density range, in the leftmost column of the lowermost row. Note that the vertical and lateral directions of each pattern correspond to a vertical movement and/or subscanning direction of the printing paper, and a lateral head heating member alignment and/or main scanning direction, respectively. The energy supply level of the heating member is varied in each pattern in accordance with a gradation signal, as in the first embodiment. In the low density range, the size (diameter) of a dot pattern transferred to the printing paper is changed in accordance with a change in the energy supply level of the heating member, thus also changing the density. In the medium density range, the size (width) of a stripe pattern transferred to the printing paper is changed in accordance with the change in the energy supply level of the heating member, thus also changing the density. In the high density range, an area of a 2×2 dot white portion other than an L-shape is changed in accordance with the change in the energy supply level of the heating member. In this case, the optical density ranges which can be indicated by changing the energy supply level of the heating member, partially overlap each other. A lower curve in FIG. 5 indicates characteristics of the discrete dot pattern of FIG. 4A, a middle curve in FIG. 5 indicates characteristics of the stripe pattern of FIG. 4B, and an upper curve in FIG. 5 indicates characteristics of the L-shaped pattern of FIG. 4C.
FIG. 6 shows an energy supply level of each dot corresponding to each halftone gradation level. In the second embodiment, the overall density is divided into 31 levels, the discrete dot pattern represents 0 to 4 halftone gradation levels (optical density), the stripe pattern represents 5 to 14 halftone gradation levels, and the L-shaped pattern represents 15 to 30 halftone gradation levels. In this manner, according to the second embodiment, a pixel of a 3×3 dot matrix can provide 31 levels. In a conventional area modulation method such as a DITHER method, a pixel of a 3×3 dot matrix can provide only 10 levels. Therefore, the number of gradation levels can be greatly increased in the present invention.
Each dot pattern used in the second embodiment has the following advantages.
(1) The dot pattern including a stripe perpendicular to a dot array of the printing head (which is constituted by a heating member array aligned along a lateral direction of the printing paper) can print a smooth pattern. The predetermined dots are continuously energized, such that the gradient of heat-diffusion becomes steep and the edge of the printed pattern becomes stable.
(2) Since each dot pattern has a white portion of 2×2 dots or more, a portion to be whitened cannot be arbitrarily blackened, and stable gradation with less noise can be obtained. This performance was confirmed by a head having a resolution of up to 16 dots/mm.
(3) When an energy supply level is changed in the same dot pattern, the printing density increases linearly with respect to an increase in the average energy per dot. That is, the density can be controlled in an analog manner. If the number of control levels are enlarged, a large of gradation number can be obtained.
(4) In advantage (3), the higher the resolution of the printing head becomes, the weaker a pattern dependency becomes. Therefore, density characteristics cannot differ from their respective patterns. The energy supply level also increases linearly with respect to an optical density, even if the dot pattern s changed.
The second embodiment will be described in more detail hereinafter. Assume, for the sake of description, that a pixel has 3×3 dots. FIG. 7 is a block diagram showing the multilevel dot pattern generator 12 in detail. Gradation data (8 bits) from the gradation signal source 10 is supplied to a buffer (RAM1) 30 and a buffer (RAM2) 32. This is to complete data supply from the signal source 10 by one operation per line. If the gradation data is not supplied to buffers 30 and 32, since the gradation data only gives one level to a pixel of 3×3 dots, the same gradation data from the signal source 10 must be supplied three times per every line. the buffers RAM1 and RAM2 have a capacity of 8 bits×854. Note that the printing head is a 2,560-dot head having 2,560 heating members aligned along the main scanning direction (since the printing paper is moved along the vertical direction in this case, the main scanning direction corresponds to the lateral direction of the paper). Since a pixel has 3×3 dots, bits of the smallest integer larger than 2,560/3, i.e., 854 bits are required. The two buffers 30 and 32 allow for high speed printing. Data in the first line (three lines in practice, because a pixel has 3×3 dots) is written into the buffer RAM1, and the data in the next line is written into the buffer RAM2. Data in the following lines are alternately written into the buffers RAM1 and RAM2. Thus, while data is written into one buffer, data can be read out from the other buffer. When data write of one line data in the buffer RAM1 or RAM2 is completed, the buffer RAM1 or RAM2 is set in a standby state. When printing of 3 line data constituting a pixel is completed, a data readout signal RAM1RD or RAM2RD is generated, and the data at the second line is read out from the buffer RAM1 or RAM2. Thereafter, this operation is repeated until printing for one page is completed (in the case of color printing, until printing for one color is completed). Assuming that a printing cycle is 2 msec/line, it requires 6 msec to read out data of one pixel line.
The same dot pattern is generated three times from the buffers RAM1 and RAM2. In reponse to the signal RAM1RD, data in the buffer RAM1 is read out, and the readout data is supplied to a multilevel dot pattern generator ROM 34. (The generator 34 can comprise a RAM.) Multilevel dot pattern data (6 bits) in the ROM 34, indicated by the input data, an output from a line counter 36 (2 bits) and an output from a heating dot counter 38 is serially generated, and is stored in a buffer (RAMB1) 40 and a buffer (RAMB2) 42. This data indicates the energy supplied to each heating member of the printing head. The counters 36 and 38 repeatedly generate data "0", "1" and "2", indicating which data is to be read out from the 3×3 dot matrix. The buffer (RAMB1) 40 and the buffer (RAMB2) 42 have a capacity of 6 bits×2,560, and are provided for two lines for the purpose of high speed driving. Data for one line (854 words) is read out from the RAM1, and is converted into dot pattern data indicating an energization energy level. When all the data (2,560 words) are written in the RAMB1, the RAMB1 is switched to the standby state. During this operation, data is read out from the other RAMB2 so as to perform one line printing.
FIGS. 8A to 8H show the above operation as a timing chart.
FIG. 9 is a detailed block diagram of the driver 14 shown in FIG. 1. It should be noted that a thermal head 16 is driven by two phases, and has two identical circuits with suffix numbers 1 and 2. The data supplied from the generator 12 is supplied to a shift register 50-1, and the output from the register 50-1 is transferred to a shift register 50-2. The same clock signal is supplied to the registers 50-1 and 50-2. The outputs from the registers 50-1 and 50-2 are supplied to latches 52-1 and 52-2 in parallel. The latches 52-1 and 52-2 receive a common latch signal. The outputs from the latches 52-1 and 52-2 are supplied to gates 54-1 and 52-2, respectively. The gates 54-1 and 54-2 receive enable signals EN1 and EN2, respectively. The outputs from the gates 54-1 and 54-2 are supplied to the heating members in respective phases of the thermal head through drivers 56-1 and 56-2.
FIGS. 10A to 10G are timing charts showing the operation of this circuit. When 2,560 bit data is serially transferred six times within 2 msec, the transfer rate is about 8 Mbits/sec. On the other hand, a thermal head drive IC normally has a transfer rate of about 4 Mbits/sec. Therefore, parallel data input ports must be provided to the thermal head for high speed data transfer. In this embodiment, the thermal head has eight inputs. Therefore, data transfer of 2,560/8 =320 bits is performed.
In this embodiment, as shown in FIG. 1, heat from the thermal head 16 is detected, and the detection data is fed back to the driver circuit 14. Since an ink amount differs depending upon the temperature of the head 16, even at the same energy level, the energy level must be controlled by heat from the head 16. For this reason, assuming that, as shown in FIG. 11, the energy level at a normal temperature (Tn) is 100%, the energy level is decreased as temperature increases. Therefore, even if the temperature is changed, a constant amount of ink can be transferred. In this embodiment, as shown in FIG. 12, the head 16 is connected to a thermistor 62, and the output therefrom is supplied to the driver 14 through an A/D converter 64.
The driver 14 exerts control, in accordance with the detected temperature value, in the following manner. As shown in FIGS. 9 and 10, energy supplied to the head 16 is controlled by the gates 54-1 and 54-2. For this reason, pulse widths of the enable signals EN1 and EN2 shown in FIGS. 13A and 13B and supplied to the gates 54-1 and 54-2, are decreased as shown in FIGS. 14A and 14B, respectively, thus serving to reduce the energy requirements. Alternatively, as shown in FIGS. 15A and 15B, when amplitudes of the output voltages from the drivers 56-1 and 56-2 are decreased, this too can decrease the energy requirements.
Another embodiment will be described in which selection of a dot pattern in each density range is altered. In a third embodiment, a dot pattern comprising a combination of L-shaped dot patterns is used in every density range. Effectiveness of the L-shaped pattern will be explained with reference to FIGS. 16A to 16C. FIG. 16A shows a concentrated pattern used in a DITHER method, FIG. 16B shows a stripe pattern and FIG. 16C shows the L-shaped pattern according to the third embodiment. Each pattern has 4 dots. Broken lines and alternate long and short dashed lines respectively indicate the sizes of pixels formed when these patterns are energized so as to transfer an ink. Note that the alternate long and short dashed lines indicate cases having higher energy. In general, in high-speed thermal transfer printing, a pixel slightly expanded along the subscanning direction (the direction in which the printing paper moves; the vertical implied in the figure) is apt to be formed. Therefore, a pixel is expanded in accordance with the number of dots along the subscanning direction. In other words, if the same amount of energy is supplied, the dynamic range of gradation is widened. In addition, since a dot generally has a regular rectangular shape and is of a small matrix size, e.g., the concentrated pattern shown in FIG. 16A, a bridge is formed between two adjacent dots when the energy level is increased, resulting in degradation in smoothness due to uneven density, and in image quality due to noise caused by the random generation of bridges. In contrast, in the L-shaped pattern shown in FIG. 16C, since the pixel is expanded within a region surrounded by dot arrays along the main scanning and subscanning directions, a wider dynamic range of gradation can be obtained as compared to the patterns shown in FIGS. 16A and 16B. This result is more notable in a pattern comprising a combination of L-shaped patterns than in a single L-shaped pattern.
FIGS. 17A to 17F show the sizes of pixels when cross-shaped patterns, as a combination of L-shaped patterns arranged in a 4×4 dot matrix, and high, medium and low levels of energy are supplied to dots. FIG. 17A shows a case wherein low level energy is supplied to the dots, and FIG. 17B shows the resultant size of a pixel. FIG. 17C shows a case wherein medium level energy is supplied to the dots, and FIG. 17D shows the resultant size of a pixel. FIG. 17E shows a case wherein high level energy is supplied to the dots, and FIG. 17F shows the resultant size of a pixel. In this manner, since the cross-shaped pattern includes four regions surrounded by dot arrays along the main and subscanning directions, the dynamic range of gradation can be widened.
In the third embodiment, it is considered that adjacent patterns should have less, and preferably no dots contacting each other when each pattern is selected. When there are no dots contacting each other between two adjacent patterns, the following effect can be obtained. As shown in FIG. 18A, cross-shaped patterns having five dots are arranged in four adjacent 4×4 dot matrices. These patterns have no dots contacting each other. FIG. 18B shows a case wherein an ink is transferred using these patterns. Since the patterns are spaced apart from each other, even if the energy level is changed, the respective patterns are kept separate. As the energy level is increased, the pixels are enlarged. However, since non-energized dots are present between adjacent patterns, attachment of an ink and ink transfer to the printing paper are unlikely to occur at such non-energized dots when peeling of the ink ribbon from the printing paper. Thus, independency of the patterns can be maintained. In this case, since the narrowest portions of the cross-shaped patterns are adjacent to each other, they serve to maintain the independency of the patterns. Even if the respective patterns contact each other, when the narrowest portions of the patterns contact each other, the center of the cross-shaped pattern is furthest from the contacting portion. Thus, pixels are expanded from the center of the dot matrix in accordance with the energy level, and non-transferred ink portions are concentrically contracted. Thus, if the energy level is increased, a satisfactory image quality can be maintained. In general, when adjacent patterns contact each other, an increase in the ink transfer area is observed in the contacting portion in accordance with pixel forming energy, this increase occurring abruptly. For this reason, linearity of gradation in accordance with an increase in pixel forming energy is often impaired.
FIGS. 19A to 19N show examples of dot patterns used in the third embodiment in the order from lower gradation levels to higher gradation levels. Note that although each pattern has 4×4 dots, it needs to have 2×2 dots or more. However, in order to print a halftone image at high resolution, m and n of an m×n matrix size satisfy, preferably, 2≦m≦n≦6. FIG. 20 shows patterns when m =n =2.
FIG. 21 shows halftone gradation levels of the third embodiment and energy supply levels for dots of dot patterns. In this case, the L-shaped pattern shown in FIG. 19A is assigned to the low density range, the cross-shaped pattern shown in FIG. 19E is assigned to the middle density range and the combined L-shaped pattern shown in FIG. 19L is assigned to the high density range, thereby providing 39 levels.
FIG. 22 is a graph for comparing the density characteristics of the multilevel pixels printed in the third embodiment and another previous embodiment (second embodiment). The characteristics of the third embodiment are indicated by the solid curve, and those of the other embodiment are indicated by the broken curve. In the third embodiment, as can be seen from this graph, the dynamic range of gradation can be widened, and a change in density can be obtained with good linearity. In addition, good image quality with no density irregularity can be obtained in the overall density range.
A fourth embodiment will be described hereinafter. In the fourth embodiment, dot patterns in each dot range are selected so that positions of the dot arrays forming each dot pattern are the same (or in the same phase). That is, the pattern is determined so that the dot array forming the pattern is located at the same position in at least one of the main and subscanning directions. This is because pixels can be stably formed since the heat pile-up of the dot can be effectively utilized, and, in each pattern, the dynamic range of gradation is wide and linearity is high.
The patterns of the fourth embodiment will be described with reference to FIGS. 23A to 23D, and FIGS. 24A to 24D for the purpose of comparison with conventional patterns. FIGS. 23A to 23D, show the conventional patterns, and, FIGS. 24A to 24D show the dot patterns of the fourth embodiment. In this case, the overall density range is divided into four ranges. FIG. 25A is a view showing a dot pattern in which the conventional patterns shown in FIGS. 23A to 23D are continuously formed. FIG. 25B is a view showing a dot pattern in which the dot patterns of the fourth embodiment shown in FIGS. 24A to 24D are continuously formed. As shown in FIGS. 23A to 23D, when positions of the crossing points of the dot arrays in the patterns are different from each other, and when different patterns are formed adjacent to each other as shown in FIG. 25A, each dot may either make contact with the adjacent dot array, or be greatly separated therefrom. Therefore, the printing state becomes that as shown in FIG. 26A. In this state, printed and blank portions are aligned irregularly, and image quality is degraded by unstable gradation production caused by noise due to uneven density or a bridge irregularly generated between dot arrays of adjacent pixels. In contrast to this, according to the fourth embodiment, as indicated by broken lines in FIGS. 24A to 24D, since the phases of dot arrays in all the patterns coincide with each other in the main scanning and subscanning directions, heating centers also coincide with each other. As shown in FIG. 25B, even when different patterns are formed adjacent to each other, all the dot arrays can be regularly aligned. For this reason, since the printed and blank portions are aligned regularly in the printed state shown in FIG. 26B, image quality will not be degraded by unstable gradation reproduction caused by noise due to uneven density or a bridge irregularly generated between dot arrays of adjacent pixels. Therefore, the gradation reproduction characteristics can be greatly improved. When pixels are regularly aligned in a matrix form on the overall printing screen and the gradation reproduction characteristics are good even in a portion in which different patterns are formed adjacent to each other, high image quality printing can be achieved with less noise as compared to a conventional method.
FIGS. 27A to 27D, FIGS. 28A to 28D and FIGS. 29A to 29D show various examples of the dot pattern of the fourth embodiment. These figures show combinations of patterns in the respective density ranges. In FIGS. 27A to 27D, positions of dot arrays coincide with each other along the main scanning direction (lateral direction in figures). In FIGS. 28A to 28D, positions of the dot arrays coincide with each other along the subscanning direction (vertical direction in figures). In FIGS. 29A to 29D, the positions of the dot arrays coincide along both the main scanning and subscanning directions.
In the case of a discrete dot pattern constituting a single dot, although a dot position can be arbitrary, if such a discrete dot is regarded as a dot array and is aligned along an extending line of a dot array in another pattern, a better effect is obtained.
A fifth embodiment will be described hereinafter. In the fifth embodiment, as shown in FIG. 30, the heating center of each pixel coincides with the center of a dot matrix, and the dot pattern is established so as to be rotation symmetrical (of 180 degrees) about the center of the dot matrix. Each pixel has a 3×3 dot matrix configuration. A discrete dot pattern having only a central dot is assigned to the low density range, as shown at the left side of FIG. 30. A stripe dot pattern having 3 dots included in the central line is assigned to the middle density range, as shown in the central portion of FIG. 30. A cross-shaped dot pattern having 5 dots included in central vertical and lateral arrays is assigned to the high density range, as shown at the right of FIG. 30. With these patterns, as shown in FIG. 31, when the gradation patterns are switched from a high to a low level or vice versa, the dot pattern nearest the switched pattern remains the same. In contrast, in the case of the use of the non-symmetrical pattern of rotation shown in FIG. 32, when the gradation patterns are switched from a high to a low level or vice versa, the dot pattern nearest the switched pattern changes, as shown in FIG. 33. In the case of FIG. 33, the dot X2 does not have the cooling interval of a blank dot; consequently the dot X2 is printed as a large dot due to a heat pile up and has a size different from the dot X1 which has a cooling interval. Furthermore, since the dot X3 has a sufficient cooling interval, it is printed as a small dot. In the case of the figure to the left in FIG. 33, the density at a boundary becomes lower than a predetermined density, and, in the case of the figure to the right, the density at a boundary becomes higher than the predetermined density, i.e., exhibits a kind of edge emphasis characteristic resulting in discontinuity in the density. In contrast to this, in the case of FIG. 31, since dots X4 and X5 have the cooling interval of blank dots, they can be printed as dots having substantially the same size.
FIGS. 34 and 35 are modifications of the dot patterns of the fifth embodiment.
A sixth embodiment will be described hereinafter. In this embodiment, as shown in FIG. 36, density ranges which are covered by respective dot patterns overlap, and the density level at which the dot patterns are switched are different in accordance with whether the density changes from a high to a low level or vie versa. In general, in the second to fifth embodiments, the dot patterns are selected in accordance with the density level and noise tends to be generated when the dot patterns are switched. For this reason, when the printing density is changed, the switching frequency of the dot patterns is preferably decreased as low as possible. In this embodiment, a changing direction of the density is detected, and when the density is changed from a high to a low level, a dot pattern which covers the high density range of the overlapping dot patterns is used. In contrast to this, when the density is changed from a low to a high level, a dot pattern which covers the low density range of the overlapping dot patterns is used. Thus, the switching frequency of the dot patterns can be reduced.
FIG. 37 shows a block diagram of the sixth embodiment. This block diagram is substantially the same as that of FIG. 1 except that a dot pattern changing controller 70 is connected between the gradation signal source 10 and the multilevel dot pattern generator 12. FIG. 38 shows the controller 70 in more detail. The gradation signal from the signal source 10 is supplied to a latch 72 and to a first input terminal of a subtractor 74 and a pattern selector 76. The output from the latch 72 is supplied to a second input terminal of the subtractor 74. The subtractor 74 subtracts the output signal from the latch 72 from the signal from the signal source 10, and supplies the subtraction result to a shift register 78. The register 78 delays an input image signal for every pixel, and outputs from the respective stages are supplied to an adder 80. The output signal from the added 80 is supplied to a latch 82, and is also supplied to a first input terminal of a comparator 84. The output from the latch 82 is supplied to a second input terminal of the comparator 84. The output from the comparator 84 is supplied to the pattern selector 76, and the output from the selector 76 is supplied to the generator 12.
With this circuit, a pixel signal delayed by one pixel by the latch 72 is subtracted from the signal from the signal source 10, and a change in density for each pixel can be detected. In order to detect a density change in the main scanning direction at equal intervals, an average value of a change in density between m pixels (m corresponds to the number of stages of the register 78) is obtained. The average value is stored in the latch 78 every m pixels, and a change in the average values is detected to be either positive or negative by the comparator 84. The output from the comparator 84 and the input gradation signal are supplied to the selector 76, and the selector 76 supplies a selection signal to the generator 12 so as to select a halftone dot pattern included in the characteristics of the low density side of two overlapping characteristics when the change in density is positive. When the change in density is negative, the selector 76 supplies a selection signal to the generator 12 so as to select a halftone dot pattern included in characteristics at the high density side.
As described above, according to the present invention, there is provided a thermal printing apparatus which can increase the number of provided density levels without increasing the number of dots of a dot matrix constituting a pixel. | A thermal transfer printing apparatus has a thermal head comprised of a plurality of heating members aligned in line, each of the heating members transferring an ink to printing paper upon heating so as to form one dot, the thermal head moving relative to the printing paper and defining a pixel using m×n printing dots (m, n: positive integers). This apparatus further has multilevel dot pattern generating means for storing several binary dot patterns having predetermined dots of the m×n dot matrix, and for selecting, upon reception of an image signal indicating the density of each pixel, a binary dot pattern in accordance with the density of each pixel, determining multilevel data for each dot constituting the selected pattern in accordance with the density of each pixel, and generating the multilevel dot pattern in which the data for each dot is determined, and driving means, connected between the multilevel dot pattern generating means and the thermal head, for heating, in correspondence with a multilevel dot pattern, the heating member corresponding to the dot therein so as to transfer an ink onto the printing paper to form a dot pattern formed by dots having a size corresponding to the density of each pixel. | 7 |
REFERENCE TO RELATED APPLICATIONS
The present application is related to U.S. patent application Ser. No. 10/653,506, entitled COMMUNICATION SESSION ENCRYPTION AND AUTHENTICATION SYSTEM, invented by Mizrah, and filed on the same day as the present application.
The present application is related to U.S. patent application Ser. No. 10/653,500, entitled KEY CONVERSION METHOD FOR COMMUNICATION SESSION ENCRYPTION AND AUTHENTICATION SYSTEM, invented by Mizrah, and filed on the same day as the present application.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates generally to security of authentication and data transmission over untrusted communication media in client-server computer, network, and other architectures, and more particularly to encryption key management systems and authentication protocols.
2. Description of the Related Art
Electronic networks of interconnected devices and users continue to grow with unprecedented rate. They have become foundations for vitally important infrastructures enabling e-commerce, communications, corporate and government operations, healthcare, education, and other important areas. This phenomenon was actively studied and commercialized during the last quarter of the 20 th century, and there is every indication this activity will intensify well into the 21 st century.
There are various parties involved in remote relationships over distributed electronic networks. Most known representations are business-to-business (b2b), business-to-consumers (b2c), and peer-to-peer (p2p), describing scaled-down to hardware devices communication, for instance, peer router to peer router, or device-to-device (d2d). One of the fundamental problems for continued growth of electronic networks and their efficient utilization is establishing trust between remote counterparts in b2b, b2c, d2d, and other interrelating over network parties. It is common knowledge that computer network intruders (or intruding organizations) cause ever-growing direct economic losses to enterprises and individual consumers. They significantly undermine the progress in applying network technologies to certain areas, especially related to parties having legal and financial responsibilities, and national security.
Trust to remote humans or devices, interacting over electronic networks, has two components. The first component is identification and verification of the parties at the beginning of the communication session (mutual authentication). The second component is associated with trust to information transferred during the communication session over untrusted communication media (communication lines). It includes the following specific requirements—confidentiality (none can read the message except the intended recipient), integrity (none altered, tampered with, or modified the message against the original), and non-repudiation (the sender cannot deny the fact of having sent the message).
Authentication and cryptography are key enabling technologies employed to satisfy the security requirements listed above. Authentication factors are typically characterized as “what user knows” (for instance, passwords, PINs), “what user has” (for instance, hardware token, smart card), and “what user is” (particular biometric traits; for instance, fingerprints, voice patterns, etc.). Passwords are the most ubiquitous over electronic networks as an authentication factor due to ease of use, low cost and easy electronic deployment. Most of the strong (two-, or three-factor) authentication systems are still using passwords or PINs as one of the system authentication factors.
However, passwords provide low security due to insufficient protection against numerous known intruding attacks on databases where the passwords are residing, social engineering attacks, videotaping or “shoulder surfing” attacks during password entry stages, memory sniffing attacks, Trojan horse attacks, and network sniffing attacks. Perhaps, the latter are the most dangerous attacks as a distributed electronic network (like Internet) has numerous access points. There are authentication systems transmitting passwords in clear text (for instance, Password Authentication Protocol (PAP) RFC 1334-2, Telnet, and FTP). Certainly, there is no protection at all in such cases. More protected authentication systems transmit encrypted passwords over electronic networks.
There are several approaches in transferring an encrypted password. The first one is based on the one-way encryption—calculating the password's hash value with one of the standard hashing algorithms (for example, SHA-1 Secure Hash Algorithm, FIPS PUB 180-1, Secure Hash Standard, 1995, Apr. 17, or MD5 Message Digest Algorithms, RFC 1320 and RFC 1321, April 1992, by Ronald L. Rivest) at both client and server locations. The client transmits the hashed password (of the user at the client platform) to the server, where it is compared with the password of the same client (the same user at the client platform) from the database connected to the server (typically, user passwords are already stored in password files in hashed form for database protection; that is why there is no need to perform text-to-hash encryption operation). Unfortunately, the progress in integrated circuit (ASIC, FPGA, etc.) design and manufacturing drastically reduced protection of hashed passwords, as dictionary or brute force computer processing attacks became extremely efficient. It is worthy to note that sometimes intercepting a hashed password is sufficient enough to break the system without learning the actual password.
There are more sophisticated authentication systems based on Challenge-Handshake Authentication Protocol (CHAP, for instance, RFC 1334-3, RFC 1934, RFC 2759) used by Microsoft for Windows NT remote log-in. The server (the authenticator) sends the “challenge” to the client (the peer), where the message gets encrypted using the client's (the peer's) password. Actually, the “challenge” sent to the client platform is then encrypted at the client location three times using the first seven bytes of the password's hash value as the first DES key (Data Encryption Standard and other known encryption algorithms used for data encryption and decryption described in Bruce Schneier, Applied Cryptography, Second Edition, John Wiley and Sons, Inc., at pp. 233-560, (1996)); the next seven bytes of the password's hash value used as the second DES key, and the remaining two bytes of the password's hash value concatenated with five zero-filled bytes used as a third DES key. Eventually, three 64-bit “responses” (the “challenge” encrypted with DES keys as described above) are sent back to the server (the authenticator), where they are compared with the similar outputs calculated at the server. If the values match, the authentication is acknowledged; otherwise the connection should be terminated.
Passwords (client/server shared secrets) in CHAP never enter communication lines in either form. This is a serious security advantage of this protocol. Also, CHAP prevents playback attacks by using “challenges” of a variable value. The server (the authenticator) is in control of the frequency and timing of the “challenge”. CHAP assumes that passwords are already known to the client and the server, and are easily accessible during a CHAP session. However, frequent usage of the same static encryption keys derived from a password on the client host, and applied to encrypt even random “challenge” numbers sent in clear text to the client, raises some security concerns. It provides ample opportunities for intruders, sniffing the network with the following offline computer data processing attacks.
Various modifications of client/server authentication employing a challenge/response protocol are disclosed in Bellovin et al., U.S. Pat. No. 5,241,599, Kung et al., U.S. Pat. No. 5,434,918, Pinkas, U.S. Pat. No. 5,841,871, Hellman, U.S. Pat. No. 5,872,917, Brown, U.S. Pat. No. 6,058,480, Hoffstein at al., U.S. Pat. No. 6,076,163, Guthrie et al., U.S. Pat. No. 6,161,185, Jablon, U.S. Pat. No. 6,226,383, Swift et al., U.S. Pat. No. 6,377,691, Brown, U.S. Pat. No. 6,487,667, Jerdonek, U.S. Pub. No. 2002/0095507. Some of these patents go beyond security of just only an authentication process. They explore the opportunity of utilizing challenge/response type protocols as a basis for an encryption key management system. This can extend security for the entire communication session duration, allowing for encrypted data transmission between parties once their mutual authentication is completed.
U.S. Pat. No. 5,434,918 and U.S. Pat. No. 6,377,691 applied client/server authentication based on different modifications of a challenge/response protocol to exchange secret keys (symmetric cryptography) between parties. There were attempts combining challenge/response protocols with well-known encryption key management systems. For instance, U.S. Pat. No. 6,076,163 and U.S. Pub. No. 2002/0095507 disclose versions of a challenge/response protocol utilizing an authentication and encryption key management system based on PKI (Public Key Infrastructure (Hellman et al., U.S. Pat. No. 4,200,770, and Diffie at al., IEEE Transactions on Information Theory, vol. IT-22, No. 6, Nov. 1976)), whereas U.S. Pat. No. 5,841,871 discloses a version of a challenge/response protocol integrated with Kerberos (NET, 1988; RFC 1510))—the authentication and encryption key management system.
Another approach would be encrypting passwords (either text or hash) with a secret key (symmetric cryptography) on the client side, before transmission, and then, decrypt it on the server side for comparison with the password stored in the server-connected database. Though it can be a viable solution, there are several security requirements making this approach a very difficult one to implement. The first issue is how to manage the session secret key distribution between the client and the server. Otherwise, if the secret keys are statically preset at the client and the server hosts, they become a security concern by themselves. Moreover, having static keys for numerous communication sessions makes encrypted passwords vulnerable against offline computer data processing attacks. There are protocols, not based on a challenge/response type mechanism, where authentication credentials are distributed over communication lines with help of PKI. They were disclosed in Kaliski, U.S. Pat. No. 6,085,320, Kausik, U.S. Pat. No. 6,170,058, Kaliski, U.S. Pat. No. 6,189,098, Spies, U.S. Pat. No. 6,230,269 and Volger, U.S. Pat. No. 6,393,127. Despite recognized scientific studies and long-time exposure, PKI and Kerberos authentication and encryption key management systems have not experienced a wide industry acceptance due to their complexity, cost, and mandatory requirements to trust artificial third parties (see, for instance, Gartner QA-18-7301, 13 Nov., 2002, by V. Wheatman, Public-Key Infrastructure Q&A, and DPRO-90693, 20 May, 2003, by Kristen Noakes-Fry, Public Key Infrastructure: Technology Overview; USENIX, 91, Dallas, Tex., “Limitations of the Kerberos Authentication System”, by Steven M. Bellovin and Michael Merritt). SSL (Secure Socket Layer, based on PKI protocol developed by Netscape Communications in 1994) is also known for its security deficiencies, high cost and complexity in assuring “client browser”/“Web server” encrypted communication (see, for instance, Gartner T-16-0632, 3 Apr., 2002, by J. Pescatore and V. Wheatman, and FT-178896, 15 Aug., 2002, by J. Pescatore). Hence, there is a significant interest in exploring other encryption key management systems, similar to the challenge/response authentication protocols mentioned above, for instance, Fielder, U.S. Pat. No. 6,105,133, Alegre, U.S. Pat. No. 6,199,113, and Venkatram, U.S. Pat. No. 6,367,010.
Aspects of this invention are particularly concerned with security of authentication systems and encrypted information exchange over distributed computer networks. Prior art encrypted authentication protocol implementations based on PKI, SSL, and Kerberos exhibited numerous security flaws and a prohibitive level of complexity and cost for various applications, businesses and organizations. There is a substantial need for improved and more efficient encrypted authentication protocols, addressing less complex infrastructures required, and less costly for practical implementation encryption key management systems. These improved encrypted authentication protocols should also include secure mutual authentication built into the protocols; randomly generated session secret keys; new cryptographic algorithms allowing for scalable security authentication and data encryption, and further allowing for variation based on the power of computer and network resources.
SUMMARY OF THE INVENTION
In accordance with the present invention, there are two secrets uniquely shared by either client/server pair, or authenticator/peer pair, and required for their mutual authentication. In the preferred embodiments, both secrets will suffice for a “what user knows” type authentication factor and either could be in a form of passwords or PINs, though other types of shared secrets can be used. Like other challenge/response type authentication protocols, where shared secrets are never in transit over communication lines, the protocol of the present invention does not allow shared secrets to pass through untrusted communication media. In order to avoid transmission of the shared secrets, a new encryption key management system has been integrated into the authentication protocol, becoming an essential part of the protocol itself.
The main function of this encryption key management system is a secure distribution within either client/server pair, or authenticator/peer pair of a secret session random key (the same secret key is used in symmetric cryptography to encrypt and then decrypt digital information). Successful exchange of this encryption key enables secure resolution of two fundamental tasks. First, it allows for secure transit of the protocol data over communication lines in encrypted form, permitting explicit mutual authentication of the connected parties. Second, the post-authentication stage of the communication session can use secure encryption for the data exchange, since each party has already obtained the secret session random key.
A series of new algorithms has been developed in the present invention and built into the new encryption key management system mentioned above. There is an algorithm (Time Interplay Limited Session Random Key (SRK) Algorithm (TILSA)) for generating and eventually obliterating arrays of session secret random keys. It starts long before the session begins and keeps processing these arrays during each communication session and well beyond it. At the same time, this algorithm allows concurrent communication between a number of client/server or authenticator/peer pairs with the same keys in the generated arrays (the multi-threading technology).
Another algorithm (Key Encryption/Decryption Iterative Algorithm (KEDIA)) is initialized, provided there is a request for connection. It initiates an iterative sequence of messages from the server to the client and back to the server, each containing a consecutive session secret random key, encrypted with the session secret random key preceding the encrypted one in the array, and sent to the client in the previous message. The client can decrypt any following message and obtain an intermediate session secret random key from the array, provided the client could decrypt the previous message. The iterations continue until client/server (or authenticator/peer) mutual authentication is completed, and the Final Secret Key (FSK) is exchanged between the parties. More particularly, client/server (or authenticator/peer) authentication credentials and FSK eventual high security are achieved by applying, during each cycle of key encryption at the server (and its decryption at the client platform), either of Byte-Veil-Unveil (ByteVU), Bit-Veil-Unveil (BitVU), or Byte-Bit-Veil-Unveil (BBVU) algorithms. Each of these algorithms disassembles message bytes, or bits, or both bytes and bits in combination, together at the server and reassemble them at the client according to a certain procedure, which is started with the pair's shared secret. In other words, the client/server or authenticator/peer pair employs their shared secret to first build the session “security bridge” over the untrusted communication medium until “the bridge” is believed secure enough. Then, the authentication credentials can be safely tested with ByteVU, BitVU, or BBVU algorithms at the respective counterparts for the final mutual authentication, enabling the communication session. Otherwise, if the mutual authentication is not completed, the communication session is terminated.
In one aspect of the invention, the client/server authentication protocol (Message Encrypt/Decrypt Iterative Authentication (MEDIA) protocol, which includes the encryption key management system described above), is highly resilient against session eavesdropping attacks, replay attacks, man-in-the-middle attacks, online and offline computer-processing attacks (like a dictionary attack or a brute force attack), and session hijacking attacks. Inability to successfully complete the MEDIA protocol can be regarded as intrusion detection (if there are more than just a few failed attempts from the same client caused by mistyping the entry data by a user on the client platform, or inaccurately set up hardware authentication credentials).
In another aspect of the invention, the MEDIA protocol ends up with a FSK secret key, which can be used beyond the client/server authentication protocol stage of the communication session for encrypting data in transit and decrypting it upon arrival either to the server, or to the client. Security of FSK, and authentication credentials (client/server shared secrets) are guarded by five security tiers of the MEDIA authentication protocol and can be scaled with the client and server platforms' CPU power and the network throughput. In order to enhance security, FSK, as well as the entire series of preceding FSK session iterative random secret keys of the MEDIA protocol, are never transmitted over untrusted electronic communication media in their original form, or as their hash equivalents.
In yet another aspect of the invention, the MEDIA protocol contains the encryption key management system, integrated into the protocol, represented by TILSA, KEDIA and ByteVU, BitVU, or BBVU algorithms. Their collective utilization assures randomly generated arrays of session secret keys, having limited life time and enabling efficient key encrypt/decrypt iterative messaging procedures, employing for each instance of iteration (each message encrypted on the server and decrypted on the client) a shared secret (password, PIN, or pattern) known only to the client and to the server. Moreover, the shared secrets (for instance, client and server passwords) are never transmitted over untrusted communication media in any form.
In still another aspect of the invention, the five security tiers of the MEDIA protocol provide for a message confidentiality (no one can read messages; this is increasingly true with the increased number of SRK in the TILSA and the number of message iterations in the KEDIA). Message integrity is preserved because, if an intruder altered or in some way tampered with the message in the conversion array, potentially available to an intruder while it is in transit on communication lines, then it will be impossible for ByteVU, BitVU, or BBVU algorithms to reassemble the encrypted keys or authentication credentials, either at the client or at the server. Message non-repudiation is guaranteed by the mutual authentication mechanism (the fifth security tier)—without exception only the client and the server know their shared secrets and respectively could send a message.
In a further aspect of the invention, the post-authentication part of the MEDIA session continued with FSK can also employ such message integrity control technique as encrypting with FSK the message hash, before the message is encrypted with FSK. Then the message hash can be decrypted with FSK on the receiving end, and compared with the same message, hashing it after having the message decrypted with FSK.
BRIEF DESCRIPTION OF THE DRAWINGS
Additional objects, features, capabilities and advantages of the present invention will be apparent from the following detailed description when read in conjunction with the accompanying drawings in which:
FIG. 1 is a graphic illustration of the Time Interplay Limited SRK (Session Random Key) Algorithm (TILSA) according to the present invention.
FIG. 2 is a graphic illustration of the Array of Data Encryption Keys (ADEK) branch of the TILSA algorithm according to the present invention.
FIG. 3 is a graphic illustration of the Key Encryption/Decryption Iterative Algorithm (KEDIA) according to the present invention.
FIG. 4 is a graphic illustration of the KEDIA typical message encryption at the server and its decryption at the client applying one of Byte-Veil-Unveil (ByteVU), Bit-Veil-Unveil (BitVU), or Byte-Bit-Veil-Unveil (BBVU) algorithms according to the present invention.
FIG. 5 is a block diagram of the Byte-Veil-Unveil (ByteVU) algorithm according to the present invention.
FIG. 6 is a block diagram of the Bit-Veil-Unveil (BitVU) algorithm according to the present invention.
FIG. 7 is a block diagram of the Byte-Bit-Veil-Unveil (BBVU) algorithm according to the present invention.
FIG. 8A is the Message Encrypt/Decrypt Iterative Authentication (MEDIA) protocol (the server side) according to the present invention.
FIG. 8B is the Message Encrypt/Decrypt Iterative Authentication (MEDIA) protocol (the client side) according to the present invention.
FIG. 9 illustrates the Graphical User Interface (GUI) enabling client/server mutual authentication at the client platform according to the MEDIA protocol, and a graphical illustration of the distributed protected network resources, including the authentication server, and the user base for which the MEDIA protocol is used, according to the present invention.
DETAILED DESCRIPTION
According to the present invention, there are shared secrets (several secrets are needed in strong authentication cases and also in a case of mutual authentication) between two parties attempting to establish trust over untrusted electronic communication media. Shared secrets are usually established during an account open procedure. Though the server password could be shared by the plurality of users, it is assumed, without sacrificing any generality of the disclosed authentication protocol, that the preferred embodiment of this invention is to provide a unique server password for each user. Account set/reset online automated utilities would greatly facilitate establishing uniquely personalized server and user passwords. Client/server or d2d (authenticator/peer) communication sessions would be typical cases, though the client/server protocol would remain the preferred embodiment. There are no limitations on the nature of the shared secrets used. They could be “what user knows” secrets, for example, passwords, or “what user has” secrets, i.e., tokens and smart cards, or, alternatively, “what user is” secrets, for example, biometrics. However, the preferred embodiments would relate to secrets in the category of “what user knows”. Also, there are no limitations on the network layer over which the authentication protocol is established—it could be TCP/IP stack, IPsec, or other communication protocols. Nevertheless, the preferred embodiments will assume HTTP (RFC 2068 Hypertext Transfer Protocol—HTTP/1.1 January 1997). Also, the invention implies contemporary object-oriented software technologies like Java, C++, and NET, providing multi-threading, serialization, servlet and applet techniques, library of cryptographic algorithms, GUI (Graphical User Interface) capabilities, and connectors/drivers like JDBC to standard commercial databases.
FIG. 1 is a graphic illustration of the Time Interplay Limited SRK (Session Random Key) Algorithm (TILSA) according to the present invention. Before any communication session starts, the server-placed logic continuously and periodically generates (Session Random Key Generator 1005 ) an array (Array of Session Keys (ASK) 1013 ) of Session Random Keys (SRK) 1011 —secret keys (symmetric cryptography). Each key has two different lifetimes. The first lifetime (LT 1 ) is the lifetime for establishing a client/server communication session, provided there is a request from a client or plurality of clients (Client 1 1003 , Client 2 1007 , . . . , Client N- 1 1008 , and Client N 1009 ) during LT 1 to initiate a communication session. Each client can establish a communication link 1015 , 1006 , . . . , 1016 , 1017 to Web Server 1002 and Compute/Applications Server 1001 through communication network 1004 . The beginning of LT 1 1014 is synchronized with each SRK 1011 generation, placing it into ASK 1013 .
For instance, in FIG. 1 , SRK 1 appears in ASK 1013 at the time mark “0 minute”, and at the moment that time mark 1 minute LT 1 of SRK 1 has expired, though SRK 1 remains inside ASK 1013 . SRK Generator 1005 at this moment generates SRK 2 and places it into ASK 1013 . By the time mark 2 minutes SRK 2 LT 1 has expired, even though SRK 2 remains inside ASK 1013 . Again, at this time SRK Generator 1005 generates and places into ASK 1013 SRK 3 , which LT 1 becomes expired at the 3 minutes mark. This procedure is periodically repeated as long as SRK Generator 1005 is on. Client 1 1003 and Client N 1009 made a connection request during the time interval between time mark 4 minutes and time mark 5 minutes, since SRK Generator 1005 began generating SRK 1011 and filling them into ASK 1013 . The only SRK 1011 not yet expired LT 1 in ASK 1013 during this time interval is SRK 5 . Therefore, SRK 5 is used to establish communication sessions with these clients. Similarly, Client 2 requested a communication session between time mark 8 minutes and time mark 9 minutes, whereas Client N- 1 requested a communication session between time mark 1 minute and 2 minutes. Hence, the SRK 1011 used to establish these communication sessions are, respectively, SRK 9 and SRK 2 .
Once LT 1 is expired, the server generates and places into ASK 1013 another SRK 1012 , which LT 1 is just started. SRK 1011 second life time LT 2 defines the life time inside the limited size ASK 1013 . The maximum size of ASK 1013 can be characterized with the parameter Nmax which indicates maximum number of SRK 1011 in ASK 1013 possible (for instance, Nmax=5 in FIG. 1 ). Typically, LT 1 <LT 2 , and in the most preferred embodiment LT 1 can be derived as LT 1 =LT 2 /Nmax. Without sacrificing any generality limitations of TILSA, LT 2 was chosen, for example, to be equal to 5 minutes in FIG. 1 . Then, LT 1 according to the formulae presented above, is equal to 1 minute. After LT 1 expired, for any given SRK 1011 , the key has LT 2 −LT 1 time remaining to support communication session threads having been initiated during LT 1 . Once LT 2 expired, SRK 1011 is removed from ASK 1013 , effectively canceling any further participation of this particular SRK 1011 in the parties' communication session engagements. Certainly, each SRK 1011 can be used to originate multiple threads of communication sessions with each Session Elapsed Time (SET) less or equal to LT 2 −LT 1 . However, SET=LT 2 −LT 1 is the preferred embodiment. Without sacrificing any generality limitations of TILSA, SET=4 minutes in FIG. 1 . Taking SRK 5 in FIG. 1 as an example of any SRK 1011 genesis, one can note that SRK 5 is the last key to fulfill ASK 1013 to its maximum size Nmax=5, and SRK 5 appears inside ASK 1013 at the 4-minute mark, since SRK Generator 1005 began generating SRK 1011 and filling them into ASK 1013 . Then, during SRK 5 LT 1 =1 minute, the key can be engaged into initiating multiple communication session threads with the clients requesting connections. From time mark 5 minutes, and until time mark 9 minutes, SRK 5 , in accordance with SET=4 minutes, is kept inside ASK 1013 available to support communication session threads started during SRK 5 LT 1 . During this particular time interval, from time mark 5 minutes to time mark 9 minutes, SRK 1 , SRK 2 , SRK 3 , and SRK 4 in ASK 1013 are being gradually replaced every minute by SRK 6 , SRK 7 , SRK 8 , and SRK 9 , respectively. Eventually, at time mark 9 minutes SRK 5 is canceled, ultimately being replaced by SRK 10 .
This Time Interplay Limited SRK Algorithm (TILSA) is the first security tier of the authentication protocol, assuring supply of SRK 1011 to initiate any client/server communication session. However, the time to initiate a session (approximately one minute, without sacrificing any generality limitations of TILSA) and the time to continue the session authentication protocol (possibly several minutes, without sacrificing any generality limitation of TILSA) are quite limited for any given SRK 1011 , thus hindering a possible intruding activity.
FIG. 2 is a graphic illustration of the Array of Data Encryption Keys (ADEK) branch of the TILSA algorithm according to the present invention. The essential part of TILSA is generating (Data Random Key Generator 2005 ) an array of Data Random Keys (DRK) 2013 —secret keys to support the authentication session for any particular SRK 1011 starting a communication session thread. This array of DRK (Array of Data Encryption Keys (ADEK) 2012 ) is regenerated and specifically attributed to each SRK 1011 , together and concurrently with originating any new SRK 1011 with the logic located on the server side; explaining why there is no latency in the DRK supply during a client/server encrypted authentication session. The number of DRK 2013 in ADEK 2012 is fixed, acting as a security parameter for the MEDIA authentication protocol being presented. Each ADEK 2012 can be used for a plurality of threads initiated with a particular SRK, to which this ADEK 2012 belongs. The ADEK 2012 lifetime is limited and equal to the lifetime of the originated SRK 1011 in ASK 1013 , being LT 2 . Deleting SRK 1011 from ASK 1013 inevitably deletes ADEK 2013 , corresponding to this SRK 1011 .
Once the client requested a connection to the server supported by the user name of the user on the client platform (or the client host name), a suitable SRK 1011 , accompanied by LT 1 , not yet expired, is sent to the client by the server. In the most preferred embodiment of this invention, SRK 1011 is sent to the client in a compiled form (for example, as a class file). This is the second security tier of the authentication protocol, in view of the fact that reengineering a compiled key given a short SRK 1011 lifetime LT 2 is a formidable task. Therefore, the first two security tiers make SRK 1011 quite resilient to the on line attacks during the session time, because of incommensurate times to reengineer SRK 1011 versus SRK 1011 expiration time LT 2 . However, SRK 1011 is still vulnerable against off line attacks and needs to be enhanced further to avoid any loss of authentication credentials and the eventual session Final Secret Key (FSK).
Since SRK 1011 is sent to the client as the first message, the logic located on the server and on the client sides generates a series of messages having been sent from the server to the client, and back to the server with the following Key Encryption/Decryption Iterative Algorithm (KEDIA). FIG. 3 is a graphic illustration of the Key Incryption/Decryption Iterative Algorithm (KEDIA) according to the present invention. In step 1 3005 , client 3002 sends a connection request to server 3001 over communication network 3003 . In step 2 3006 , SRKi (with the currently active LT 1 i —between time mark i−1 minutes and time mark i minutes) is sent to client 3002 , and stored there, initiating the communication interface. In step 3 3007 , client 3002 enters the user name, the user password, and the server password, if it is a user at the client platform 3002 , or the host name, the host ID, and the server password, if it is the client platform (the peer). In step 4 3008 , the user name (or the host name) is hashed, encrypted with SRKi and sent to server 3001 , while the user password (or the host ID) and the server password were not sent, remaining at client 3002 .
In step 5 3009 , server 3001 checks the validity of the user name (or the host name), obtained in the step 4 , through the database to which it is connected. The session is terminated, if the user name (or the host name) is not valid. Otherwise, server 3001 in step 3009 sends DRK 1 encrypted with SRKi to client 3002 , where DRK 1 is decrypted with SRKi, and stored at client 3002 . During the same step 3009 , client 3002 sends a DRK 1 , which is converted to its hash equivalent and encrypted with DRK 1 , to server 3001 . This message confirms to server 3001 that client 3002 obtained and decrypted DRK 1 , and it is ready for receiving another secret key. In step 6 3010 , server 3010 first decrypts hashed DRK 1 , received in step 5 from client 3002 , with DRK 1 . If DRK 1 is correct, server 3001 sends DRK 2 encrypted with DRK 1 to client 3002 , where DRK 2 is decrypted with DRK 1 , and stored at client 3002 . Otherwise, the communication session is terminated. During the same step 6 3010 , client 3002 sends a DRK 2 , converted to its hash equivalent, and encrypted with DRK 2 , to server 3001 . This message confirms to server 3001 that client 3002 obtained and decrypted DRK 2 , and it is ready for receiving another secret key.
This iterative process continues up to step n 3014 . Parameter n is actually the maximum number of DRK 2013 in ADEK 2012 ( FIG. 2 ), and should be chosen for any practical implementation of this encrypted authentication protocol. Then, assuming DRKn−1 hash received from client 3002 in the previous step n−1 is correct, server 3001 , sends DRKn, encrypted with client 3002 hashed password (taken from server database 3004 , as server 3001 knows from step 4 3008 , the identification of the client (or the user on the client platform)) to client 3002 , where DRKn is decrypted with the client 3002 password, stored at the client side in step 3 . During the same step n, client 3002 sends to server 3001 hashed DRKn encrypted with the client 3002 password, stored at client 3002 at step 3 and converted to its hash equivalent. Step n is an important first phase towards client/server mutual authentication. Indeed, the client can decrypt DRKn only in the case where client 3002 knows the user 3002 password. Then, client 3002 encrypts hashed DRKn with the client 3002 hashed password, as a secret key and sends it back to server 3001 in same step n 3014 . Having received DRKn encrypted with client 3001 password, server 3001 decrypts it with the client 3001 password, and, if it is correct, server 3001 , in step n+1 3015 , sends to client 3002 DRKn encrypted with hashed server 3001 password as a key.
Certainly, client 3002 , already aware of DRKn from the previous step n 3014 , compares the result of decrypting the last message with the server 3001 password, stored at client 3001 in step 3 3007 , and converted to its hash equivalent, with DRKn. If they are the same, the client is assured that the communication session is with the correct server, as only client 3002 and server 3001 know the server 3001 password. Otherwise, the client 3002 terminates the communication session, and intrusion detection is reported. Eventually, during same step n+1 3015 , client 3002 sends to server 3001 hashed DRKn encrypted with the server password, stored at client 3002 , at step 3 3007 , and converted to its hash equivalent. This message, transmitted back to server 3001 , means that client 3002 has established trust to server 3001 . In step n+2 3016 , server 3001 decrypts hashed DRKn with the server password from the 3004 database connected to the server, and compares the result with DRKn at server 3001 . Depending on the comparison results, server 3001 , during same step n+2 3016 , sends to client 3002 the authentication signal “go/no” encrypted with DRKn−1, stored at client 3002 , at the step, prior to step 3014 . This completes the client/server mutual authentication and Final Secret Key (FSK) exchange according to the KEDIA algorithm.
One encryption/decryption algorithm used in an embodiment of the invention is the Triple Data Encryption Standard block cipher algorithm. Triple-DES (3DES), based upon the Triple Data Encryption Algorithm (TDEA), is described in FIPS 46-3. Other block cipher algorithms are also suitable, including RC6, Blowfish/Twofish, Rijndael, and AES. See, Bruce Schneier, Applied Cryptography, Second Edition, John Wiley and Sons, Inc., cited above.
In this form the KEDIA algorithm, described above as part of the authentication communication protocol, is the third security tier, efficient against online and offline intruding attacks. Among other factors, the security against online attacks is increased due to effectively extending the time, needed by an intruder to decrypt the entire series of DRK 2013 in ADEK 2012 , whereas the ADEK 2012 life time is quite limited and is actually equal to LT 2 , the same as for SRK 1011 , which originated this ADEK 2013 . As mentioned above, the number of DRK 2013 in ADEK 2012 is the authentication protocol security parameter and can be chosen according to the security requirements, considering the actual system CPU and network resources. Security against offline attacks is assured through the mutual client/server authentication utilizing shared secrets known only to the client, and to the server. Moreover, the client supposed to perform a strong (two factors) authentication, as the KEDIA algorithm requires the client to enter correctly the client (the user on the client platform) password and the server password, unique to the client (the user on the client platform). Important security feature of the KEDIA algorithm are (1) that client/server passwords never enter communication lines in either form, (2) client/server pair performs mutual authentication in steps n 3014 , n+1 3015 , and n+2 3016 , and (3) client/server pair exchanges FSK enabling transmitted data encryption during the post-authentication stage of the communication session.
In the case where an intruder intercepts the last message in step n+2, and somehow knows the format of the “go/no” authentication signals, a brute force computer processing attack could be applied to uncover DRKn−1. However, the intruder would only gain limited access as DRKn−1 is detached from client/server authentication credentials, and from DRKn (which is FSK in this particular embodiment of the KEDIA algorithm).
Therefore, an offline attack is senseless, as the intruder going backward through steps 3013 , 3010 , 3009 , and 3008 could find DRKn−2 DRKn−3, . . . , DRK 1 , and eventually SRKi, which are all only one-time session random keys, and they cannot be reused. Certainly, the intruder could further decrypt the user name; however, this is not regarded as a secret. The time DRKn−1, operating during the client/server communication session, is excruciatingly small for attempting an online computer processing attack. Even assuming this attack successful, all, the intruder could do is to send to client 3002 an incorrect authentication signal, which will be visualized in the user's session GUI, but would never take effect in the actual system. This is because the authentication signal “go/no” enables functionality through the server 3001 side logic.
The KEDIA algorithm security has been further significantly enhanced by integrating and synthesizing it with the Byte-Veil-Unveil (ByteVU) algorithm, the Bit-Veil-Unveil (BitVU) algorithm, and the Byte-Bit-Veil-Unveil (BBVU) algorithm. All three algorithms are built around the idea that every encrypted message in the client/server dialogue in the KEDIA algorithm is a fixed byte size, relatively small (typically 16 bytes) message. The algorithms employ the fact that the server already has identified who the client pretends to be, after receiving the user name (or the host name) during the initial connection request. At this time, the server finds the password, or another shared secret, corresponding to the user name (or the host name), in the server database 3004 , connected to the server. Then, the server employs this information to disassemble only message bytes, or only bits, or the combination thereof, inside a certain conversion array, making their reassembling a highly improbable task, unless the client knows the shared secret. In this case, the message, which is the encrypted key, is easily recovered and eventually decrypted with the secret key, learned from the previous message.
FIG. 4 is a graphic illustration of the KEDIA algorithm. This is a typical message encryption at the server and its decryption at the client, applying along with encryption and decryption procedures one of Byte-Veil-Unveil (ByteVU), Bit-Veil-Unveil (BitVU), or Byte-Bit-Veil-Unveil (BBVU) algorithms, according to the present invention. Step 6 3010 has been chosen as a typical message example in the KEDIA algorithm. According to FIG. 3 , during this step, server 3001 sends DRK 2 encrypted with DRK 1 to client 3002 , where DRK 2 is decrypted with DRK 1 , received by client 3002 in the previous step 3009 from server 3001 . In FIG. 4 , step 3010 is split for clarity into two parts 4001 and 4002 , which are related to preparing the message at server 3001 , and treating the received message at client 3002 , respectively. Blocks 4003 , 4005 , 4007 , and 4009 depict the process the message is going through, before it is sent to client 3002 . DRK 2 (for instance, 16 bytes long, secret key to be used with a block-cipher encryption algorithm) is supplied by Server DRK Generator 2005 (see FIG. 2 ) 4003 . In the following step 4005 , server 3001 , already having identified who claims to be the user on the client platform, (or what is the claimed client platform host name), extracts the respective user password (or the client host ID) from the database 3004 attached to server 3001 . Eventually, according to block 4007 , server 3001 uses this information to trigger operation of one of ByteVU, BitVU, or BBVU algorithms, having been chosen by a particular security system, considering security requirements vs. cost trade-offs (time of operations, CPU power of client/server platforms, and the network throughput). As a final result 4009 , the conversion array, containing disassembled DRK 2 bytes, or bits, or the combination thereof, gets encrypted with DRK 1 , and sent to client 3002 .
Part 4002 of step 3010 , related to the received message treatment at client 3002 , is expanded by the series of blocks 4004 , 4006 , 4008 , and 4010 in FIG. 4 . According to block 4004 , client 3002 decrypts the conversion array with DRK 1 , stored by client 3002 from the previous message 3011 from server 3001 . Then, client 3002 supplies the user password (or the client host ID) which was entered into the KEDIA algorithm at step 3 3007 (see FIG. 3 ), enabling reassembling of DRK 2 from the decrypted conversion array 4006 . As it is shown in block 4008 , the operation is triggered for one of ByteVU, BitVU, or the BBVU algorithms, having been chosen on the client side the same one, as on the server side. Eventually, according to block 4008 , either the message bytes, or bits, or the combination thereof, get reassembled, and finally, as it is shown in block 4010 , DRK 2 is reconstructed to its original form.
In compliance with FIG. 4 , each message of the KEDIA algorithm employs additional treatment as compared to the standard encryption/decryption operations. This treatment is triggered by the client/server shared secret at the sending and receiving communication channel ends. FIG. 5 is a block diagram of the Byte-Veil-Unveil (ByteVU) algorithm according to the present invention. Block 5001 shows DRKj, where each byte is separated from a neighboring byte with a vertical bar. Without sacrificing any generality of the ByteVU algorithm, DRKj is assumed to be a 16-bytes key in FIG. 5 . The user password (or the client host ID), supplied by server 3001 in a hashed form, plays a seed role for Server Sequential Random Number Generator (SRNG) 5002 . SRNG 5002 generates a random sequence of integers, and it is the same sequence of integers, each from 1 to 10, for any given seed. In other words, the password (or the client host ID) and the SRNG sequence of integers are uniquely associated. Block 5005 introduces a conversion array which, without sacrificing any generality limitations of ByteVU algorithm, has 16 equal sections 5006 , 5007 , 5008 , 5009 , and 5010 , with 10 bytes per each section. FIG. 5 presents an exemplary case, when SRNG 5002 generated 16 sequential integers 4, 9, . . . , 2, and 7.
The first integer 4 is used by the logic located by the server 3001 to replace byte r 1 , 4 in the first section 5006 of conversion array 5005 by the first byte xh 1 of DRKj in 5001 . Similarly, the second integer 9 is used by that same logic to replace byte r 2 , 9 in the second section of conversion array 5005 by the second byte xh 2 5012 of DRKj in 5001 . The same procedure is applied to all integers in the sequence generated by SRNG 5002 , until DRKj 15 th byte xh 15 in 5001 is replacing the 2 nd byte r 15 , 2 in the 15 th section 5009 of conversion array 5005 , and eventually DRKj 16 th byte xh 16 in 5001 is replacing the 7 th byte r 16 , 7 in the 16 th section of conversion array 5005 . Once all bytes of DRKj are veiled in this manner inside conversion array 5005 , the entire conversion array 5005 is encrypted with DRKj−1, and the message is sent to client 3002 . At client 3002 , the encrypted conversion array is decrypted with DRKj−1, saved at client 3002 , from the previous server message (step 3011 in KEDIA, FIG. 3 ).
The next procedure, reversed as compared to the procedure described above on the server 3001 side, is applied. The user password (or the client host ID) saved at the client platform in step 3007 of the KEDIA algorithm (see FIG. 3 ) is supplied in a hashed form as a seed to Client Sequential Random Number Generator (SRNG) 5003 , identical to the one on the server 3001 side. This password (or host ID) triggers SRNG 5003 to generate the same sequence of integers, as on server 3001 side before 4, 9, . . . , 2, 7. Then, the logic placed on client 3002 used the first integer 4 to extract DRKj first byte xh 1 from the fourth position in first 10 bytes section 5006 of conversion array 5005 , and place it back in the 1 st position of DRKj 5001 . Consequently, the second integer 9 is used to extract DRKj second byte from the 9 th position in 10 bytes section 5007 of conversion array 5005 , and place it back into the 2 nd byte position of DRKj 5001 . This procedure is going on, until, eventually, the 15 th byte of DRKj xh 15 is extracted from the 2 nd byte position in 15 th 10 bytes section 5009 of conversion array 5005 , and placed back into 15 th byte position of DRKj 5001 as well as the 16 th byte of DRKj xh 16 5011 extracted from the 7 th byte position in 15 th 10 bytes section 5010 of conversion array 5005 , and placed back into 15 th byte position of DRKj 5001 . This completes the reassembling procedure of the ByteVU algorithm to restore DRKj at client 3002 .
A suitable sequential random number generator SRNG for use in embodiments of the invention is a Java version of the well known “Lehmer generator.” See, Park & Miller, “Random Number Generators, Good Ones are Hard to Find,” Communications of the ACM, Vol. 31, No. 10, (1988), pages 1192-1201.
FIG. 6 is a block diagram of the Bit-Veil-Unveil (BitVU) algorithm according to the present invention. The BitVU algorithm is a natural extension of the ByteVU algorithm. Instead of veiling bytes of DRKj, the BitVU algorithm veils bits of DRKj. It is assumed, without sacrificing any generality limitations of the BitVU algorithm, that DRKj bit size is 128 bits 6001 . Each bit of DRKj in 6001 is separated from a neighboring bit with a vertical bar. Server Sequential Random Number Generator (SRNG) 6002 uses the user password (or the client host ID) supplied by the server in a hashed form as a seed, allowing for the generation of a random series of 128 integers with values ranging from 1 to 128 (for instance, 4, 127, . . . , 4, 2), and each one pointing to a DRKj consecutive bit veiled position in conversion array 6005 , respective sections 6006 , 6007 , . . . , 6008 , . . . , 6009 , and 6010 of 128 bit size each. In other words, the password (or the client host ID) and the SRNG 6002 sequence of integers are uniquely associated.
Block 6005 introduces a conversion array which, without sacrificing any generality limitations of BitVU algorithm, has 128 equal sections 6006 , 6007 , . . . , 6008 , . . . , 6009 , and 6010 , with 128 bits per each section. FIG. 6 presents an exemplary case, when SRNG 6002 generated 128 sequential integers 4, 127, . . . , 4, and 7. For this exemplary case disclosed in FIG. 6 , the 1 st bit of DRKj 6001 yh 1 is put into the 4 th bit position of first section 6006 instead of r1,4 bit; then the 2 nd bit of DRKj 6001 yh 2 6012 is put into 127 th bit position of second section 6007 instead of r2,127 bit, and so on, until 127 th bit of DRKj 6001 is put into the 4 th position of 127 th section 6009 instead of r127,4 bit. Ultimately, the 128 th bit of DRKj 6001 is put into the 2 nd bit position of the 128 th section 6010 of conversion array 6005 instead of r128,2 bit. Once all bites of DRKj are veiled in this manner inside conversion array 6005 , the entire conversion array 6005 is encrypted with DRKj−1, and the message is sent to client 3002 .
At client 3002 , the encrypted conversion array is decrypted with DRKj−1, saved at client 3002 , from the previous server message (step 3011 in the KEDIA algorithm, FIG. 3 ). Then the procedure, a reversed one as compared to that which is described above for the BitVU algorithm on server 3001 side, is applied. The user password (or the client host ID) saved at the client platform in step 3007 of the KEDIA algorithm (see FIG. 3 ) is supplied in a hashed form as a seed to Client Sequential Random Number Generator (SRNG) 6003 , identical to the one on the server 3001 side. This password (or host ID) triggers SRNG 6003 to generate the same sequence of integers as on server 3001 side before, that is 4, 127, . . . , 4, 2. Then, the logic placed on client 3002 used the first integer 4 to extract DRKj 1 st byte yh 1 from the 4 th position in 1 st 128 bits section 6006 of conversion array 6005 , and placed it back in the 1 st position of DRKj 6001 . Consequently, the second integer 127 is used to extract DRKj 2 nd bit from the 127 th position in 2 nd 128 bits section 6007 of conversion array 6005 , and place it back into the 2 nd bit position of DRKj 6001 . This procedure continues until, ultimately, the 127 th bit of DRKj yh 127 is extracted from the 4 th bit position in 127 th 128 bits section 6009 of conversion array 6005 , and placed back into 127 th bit position of DRKj 6001 , as well as the 128 th bit of DRKj yh 128 6011 being extracted from the 2 nd bit position in 128 th 128 byte size section 6010 of conversion array 6005 , and placed back into 128 th bit position of DRKj 6001 . This completes the reassembling procedure of the BitVU algorithm to restore DRKj at client 3002 .
FIG. 7 is a block diagram of the Byte-Bit-Veil-Unveil (BBVU) algorithm according to the present invention. Block 7001 shows DRKj, where each byte is separated from a neighboring byte with a vertical bar. Without sacrificing any generality limitations of the BBVU algorithm, DRKj is assumed to be a 16-bytes key in FIG. 7 . The user password (or the client host ID), supplied by server 3001 in a hashed form, plays a seed role for Server Sequential Random Number Generator (SRNG) 7002 . SRNG 7002 generates a random sequence of 16 integers, and then the server's Sequential Direct Bit Position Scrambler (SDBPS) 7006 scrambles all bit positions in the veiled byte 7010 . SDBPS 7006 generates a random series of non-repeating eight digits within the range from 1 to 8, for each of SRNG 7002 integers in the sequence. In other words, the password (or the client host ID), the SRNG 7002 sequence of integers, and the series of digits generated by SDBPS 7006 are uniquely associated. Applying the same seed (the user password, or the server host ID, in a hashed form) will result in the same sequence of integers generated by SRNG 7002 , and the same series of digits generated by SDBPS 7007 for each integer in the sequence.
Block 7006 introduces a conversion array which, without sacrificing any generality limitations of the BBVU algorithm, has 16 sections similar to 7008 , with 10 bytes per section. Similarly to the ByteVU algorithm, each section will veil one byte of DRKj 7001 in a position, respective to the particular integer value generated by SRNG 7002 . For instance, the 1 st byte of DRKj 7001 xh 1 occupies the 4 th byte position in section 7008 , replacing r1,4 byte. FIG. 7 presents an exemplary case, where the 1 st DRKj byte xh 1 has an 8-bit representation from the most significant bit xh 1 , 8 to the least significant bit xh 1 , 1 7009 , and chosen as 01011101 in FIG. 7 7009 . SRNG 7002 generated 16 sequential integers 4, . . . , while SDBPS 7006 generated a series of eight non-repeating digits 3, 1, 8, 5, 4, 2, 7, and 6 for the first integer 4 7011 , and a similar series of digits for the rest of the integers. Eventually, all bits of the 1 st DRKj 7001 byte in 7008 occupy new bit positions, consecutively specified in the SDBPS 7006 generated series of digits for the first integer 4. For a particular example in FIG. 7 7012 , it is 01011011. The same process 7013 of scrambling bits for each veiled byte of DRKj 7001 in conversion array 7007 is continued, until all bytes of DRKj are veiled, and all bit positions of each veiled byte are scrambled. Then, the entire conversion array 7007 is encrypted with DRKj−1, and the message is sent to client 3002 .
At client 3002 , the encrypted conversion array is decrypted with DRKj−1, saved at client 3002 , from the previous server message (step 3011 in KEDIA, FIG. 3 ). Then the procedure, a reversed one as compared to that which is described above for the BBVU algorithm on server 3001 side, is applied. The user password (or the client host ID), saved at the client platform in step 3007 of the KEDIA algorithm (see FIG. 3 ), is supplied in a hashed form as a seed to Client Sequential Random Number Generator (SRNG) 7005 identical to the one on the server 3001 side. This password (or host ID) triggers SRNG 7005 to generate the same sequence of integers as on server 3001 side before 4 Client Sequential Reverse Bit Position Scrambler (SRBPS) 7003 generates the reversed series of digits for each integer, as compared to its server counterpart SDBPS 7006 . For instance, for the first integer 4, SRBPS 7003 generates the reversed series 2, 6, 1, 5, 4, 8, 7, and 3, which allows the logic placed on client side 3002 to restore bits in the original order for the 1 st byte of DRKj means that the 2 nd bit of the scrambled byte will become the least significant bit in the restored 1 st DRKj byte, and so on, until 3, the last digit in the series, is reached, indicating that the 3 rd bit in the scrambled byte will become the most significant bit in the restored 1 st byte. Meanwhile, integer 4 points to the 4 th position in section 7008 of conversion array 7007 , where the 1 st DRKj byte has been veiled. The same procedure continues, until all byes of DRKj 7001 and their respective bits are returned to their original positions. This completes the reassembling procedure of the BBVU algorithm to restore DRKj at client 3002 .
At this time it is important to note that the ByteVU, BitVU, and BBVU algorithms, disclosed above, require assessment of security of these algorithms against possible computer processing attacks now and in the future. Table 1 below presents a summary of this assessment. SRNG 5002 , 5003 ( FIG. 5 ), 6002 , 6003 ( FIG. 6 ), and 7002 , 7003 ( FIG. 7 ) generate integers pseudo-randomly, as well as SDBPS 7006 and SRBPS 7003 ( FIG. 7 ). Hence, probabilities of veiling each byte and bit inside a Conversion Array (CA) for each algorithm can be viewed as independent ones. Best microprocessors achieved ˜1 GHz clock rate barrier by the beginning of the 21 st century. Previously, forecasting allowed for at least 25-35 years, until the clock rate would reach ˜(100-1000) GHz. Thus, currently available ˜1E10 instructions per second could reach ˜(1E12-1E13) instructions per second in a distant future, (assuming microprocessor RISC pipelined architecture with up to 10 stages per cycle). A very conservative assumption is made that the attacking computers have 100% efficiency of their CPU utilization during an attack. In other words, testing each possible combination of all bytes, bits, or the combination thereof, of a veiled message in CA will consume only one microprocessor instruction.
Column 1001 in Table 1 presents particular geometries of CA chosen in each algorithm for the assessment. Column 1002 gives the bit size of each algorithm CA for every geometry selected in 1001. Column 1003 presents the total number of pseudo-random integers generated by SRNG of each algorithm with respect to the geometries chosen in 1001. Column 1004 introduces probability models for each algorithm with respect to the geometries of CA chosen in 1001. Every position in 1004 gives probability to estimate the entire combination of veiled bytes, bits, or the combination thereof, for each algorithm, under given geometry of CA in 1001. Column 1005 presents for each CA its transit time, given the slowest standard modem of 28.8 kbps (kilobits per second) of contemporary networks (for example, the Internet). Column 1006 presents assessed time, required for a brute force attack now and in a distant future, for each algorithm and their respective geometries of CA chosen in 1001. Column 1007 presents an approximate time for one advanced microprocessor 1 GHz/100 GHz) instruction now, and in a distant future.
TABLE 1
1001
1002
1004
1005
1006
1007
↓
↓
1003
↓
↓
↓
↓
CA Size
CA
↓
Prob-
CA Transit
Brute Force
CPU One
# of
Total
SRNG
ability
Time
Attack
Instruction
rows vs.
Bit
total
Model
modem
Time
Time, (S)
# of BB
Size
#
for CA
28.8 kbps
Now/Future
Now/Future
ByteVU
16r/16 bytes
2048 bits
16
(1/16){circumflex over ( )}16
71 milliSec.
58 y/7 months
1E-10/1E-12
BitVU
128r/2 bits
256 bits
128
(1/2){circumflex over ( )}128
9 milliSec.
1E21 y/1E19 y
1E-10/1E-12
BBVU
16r/2 bytes
256 bits
144
((.5)(1/8){circumflex over ( )}8){circumflex over ( )}16
9 milliSec.
8E102y/8E100y
1E-10/1E-12
Summarizing the assessment results in Table 1, it can be noted that each of ByteVU, BitVU, and BBVU algorithms give extremely high security now and in a distant future for the respective geometries selected in 1001. At the same time, one CA message transit times 1005, even for the slowest standard modems, are reasonable enough for the disclosed algorithms' practical utilization in the MEDIA protocol. Certainly, geometry parameters in 1001 can be regarded as security parameters of the MEDIA protocol, and these parameter changes could allow for security trade-offs vs. cost (CPU power of client/server or authenticator/peer platforms, and the network throughput). Also, replacing slow modems by contemporary high-speed network connections, like DSL, would significantly reduce message transit times in 1005.
The combination of the KEDIA algorithm and any one of ByteVU, BitVU, and BBVU algorithms comprise the fourth security tier, which makes the encrypted authentication protocol highly secure against online and offline attacks. The algorithms described above allow for the encryption key management security to be scaled with CPU and network throughput resources. During the encryption key distribution stage over communication lines, shared secrets never leave the server, or the client. However, they are repeatedly employed for each iterative message encryption/decryption by KEDIA and any of ByteVU, BitVU, or BBVU algorithms on the server and the client platform as well. Only when the client and the server eventually have in their possession the Final Secret Key (FSK) satisfying the required security level, then the server and the client will perform mutual authentication in a way that neither of authentication credentials enter communication lines in either form. The authentication session is denied, provided the parties' mutual authentication is not successfully completed. This part of the encrypted authentication protocol completes the client/server mutual authentication. At the same time, it is the final fifth security tier of the encrypted authentication protocol.
FIG. 8A and FIG. 8B illustrate the server and the client side of the Message Encrypt/Decrypt Iterative Authentication (MEDIA) protocol according to the present invention. Without sacrificing any generality limitations of the MEDIA protocol, the exemplary case presented in FIG. 8A and FIG. 8B is assuming HTTP communication protocol (RFC 2068 Hypertext Transfer Protocol—HTTP/1.1 January 1997), Java applet/servlet multi-threading object-oriented communication technology, and a standard Web server technology. However, the MEDIA protocol can be integrated into any other network communication protocol, and enabled with various object-oriented technologies. The ByteVU algorithm has been included into the MEDIA protocol in FIG. 8A and FIG. 8B , though any of BitVU and BBVU algorithms could serve there equally well.
Messages sent to the client and received at the server are numbered in 8000 . Key functional message destinations on the server side are in 8001 , and on the client side they are in 8016 . For each message received at the server, its content description is in 8003 , whereas for each message received at the client, its content description is in 8014 . Similarly, for each message sent from the server, its content description is in 8002 , whereas for each message sent from the client, its content description is in 8015 . The choice of any one of ByteVU, BitVU, or BBVU algorithms to be used in the MEDIA protocol and the parameters of the respective conversion array are in 8006 for the server side, and in 8010 for the client side. Seeds, having been used to trigger SRNG (Sequential Random Number Generator), are in 8007 for the server side, and they are in 8009 for the client side. Which direction a particular MEDIA message is sent towards, is in 8008 . The ByteVU algorithm conversion array parameters, chosen in FIG. 8A and FIG. 8B (10 sections with 25 bytes size of each), give extremely high security protection against online and offline intruding attacks, even for one MEDIA message as it was shown above. Therefore, it is practically justifiable to reduce iterations in the KEDIA algorithm by limiting DRKn in FIG. 3 to DRK 2 only. It saves client/server platforms CPU and network resources, while keeping a very high security level.
It is assumed, without sacrificing any generality of the MEDIA protocol, that for this particular embodiment of the MEDIA protocol ( FIG. 8A and FIG. 8B ), the client is a user at the client platform. The communication session begins with the user's request (message 1 ) to the server to reach a protected network resource, for example, a URL (Universal Resource Locator), a protected link, a protected file, a protected directory, or another protected network resource. This message initiates the MEDIA protocol on the server side. The server replies to the user (message 2 ), sending SRK 1011 (see FIG. 1 ) over the communication line (the Internet) in a compiled class form, which prevents any easy key reuse or reengineering, if it is intercepted by an intruder. The user enters into the GUI (Graphical User Interface, designed into the applet and sent from the server to the client in message 2 along with the SRK) the user name, the user password, and the server password. The passwords stay stored at the client, while the user name gets encrypted with the SRK and sent to the server in message 3 .
The server (logic on the server side in this exemplary case could be implemented in the Java servlet technology) replies in message 4 with DRK 1 2012 ( FIG. 2 ) bytes veiled with the ByteVU algorithm, triggered by the server, supplying the hashed password of the assumed user as a seed. The resulting ByteVU conversion array is encrypted with the SRK and sent to the client. The client, having known the SRK and the user password, entered into the GUI in the previous message 3 , decrypts the conversion array and reassembles DRK 1 bytes. In message 5 , from the client to the server, hashed DRK 1 bytes are veiled with ByteVU algorithm, triggered by the user password, stored at the client earlier in step 3 ( FIG. 8B ), and converted to its hash equivalent. Then, the conversion array is encrypted with DRK 1 and sent to the server, which decrypts the conversion array with DRK 1 , and triggers ByteVU with the hashed password of the assumed user, taken from the database attached to the server. If the hashed DRK 1 is correct, reassembled in this way, it is actually the authentication signal from the client to the server, as nobody except the client knows the user password used to trigger the ByteVU algorithm when receiving message 4 , and sending message 5 .
If DRK 1 is incorrect, the MEDIA protocol is terminated by the server sending a “no” authentication message (or an error message: “user password is incorrect”) to the client, encrypted with SRK. Otherwise, the server sends to the client message 6 containing DRK 2 , which bytes are disassembled by the ByteVU algorithm, triggered by the user hashed password, used as a seed for SRNG 5002 ( FIG. 5 ). Then, the conversion array is encrypted with DRK 1 and sent to the client, where it is decrypted with DRK 1 stored at the client from the previous message 5 , and DRK 2 bytes get reassembled by the ByteVU algorithm, triggered by the user password, stored at the client earlier in step 3 ( FIG. 8B ). The client replies to the server with message 7 , sending to the server hashed DRK 2 , which bytes are veiled by the ByteVU algorithm, triggered by the user password, stored at the client in the previous message 3 , and converted to its hash equivalent. The server decrypts message 7 from the client with DRK 2 , and reassembles the hashed DRK 2 bytes with the ByteVU algorithm, triggered by the user password, taken from the attached to the server database, and converted to its hash equivalent. If DRK 2 is correct, the server sends to the client message 8 with DRK 2 , which bytes are disassembled with the ByteVU algorithm, triggered by the server password. Otherwise, if DRK 2 is not correct, the MEDIA protocol is terminated. The conversion array of the ByteVU algorithm in message 8 is encrypted with DRK 2 and sent to the client.
The client, receiving message 8 from the server, decrypts it with DRK 2 , and reassembles the hashed DRK 2 bytes with the ByteVU algorithm, triggered by the server password, stored on the client side in message 3 . Then, the client compares the decrypted and reassembled DRK 2 with DRK 2 from the previous message 6 . If they are the same, it is viewed by the client as the authentication signal from the server, because only the client and server share the server password. Hence, it was the only server, which could send the last message 8 to the client. Now, as the trust is established by the client to the server, the client sends to the server message 9 with hashed DRK 2 , which bytes are disassembled with the ByteVU algorithm, triggered by the server password, stored on the client side in message 3 , and converted to its hash equivalent. Eventually, the conversion array of the ByteVU algorithm is encrypted with DRK 2 and sent to the server. The server, having received message 9 from the client, decrypts it with DRK 2 , and reassembles the hashed DRK 2 bytes with the ByteVU algorithm, triggered by the hashed server password. If DRK 2 is correct, it is viewed by the server as a second authentication factor from the client (the client confirmed the server password), in addition to the first factor, having been checked in the message 6 from the client (the client confirmed the user password).
This completes the mutual authentication of the client/server pair according to the MEDIA protocol, and the server is now ready to make an authentication decision. In the end, the server sends to the client message 10 , which has either a “go” authentication signal, assuming DRK 2 in message 9 from the client was correct, or an error message: “the server password is incorrect”, assuming DRK 2 in message 9 from the client was incorrect. Each signal byte is disassembled with the ByteVU algorithm, triggered by the user password from the database, attached to the server, and then the conversion array of the ByteVU algorithm is encrypted with DRK 1 and sent to the client in message 10 . Having received the message 10 , the client decrypts it with DRK 1 , stored at the client platform during message 4 , and reassembles the signal bytes with the ByteVU algorithm, triggered by the user password, stored at the client side in message 3 .
This effectively completes the entire MEDIA protocol of the client/server communication session as presented in FIG. 8A and FIG. 8B . As one can see, authentication credentials (the user password and the server password in this particular embodiment) have never passed through communication lines in any form. Also, the client/server mutual authentication has been completed within the MEDIA protocol, as well as the exchange of FSK (Final Secret Key, which is DRK 2 in this particular embodiment) having been performed within the client/server pair. The server password and the user password enable secure mutual authentication, according to the MEDIA protocol architecture. At the same time, they are both playing a role of a strong two-factor authentication of the client at the server platform.
FIG. 9 illustrates the Graphical User Interface (GUI) enabling client/server mutual authentication at the client platform according to the MEDIA protocol, and a graphical illustration of the distributed protected network resources, including the authentication server, and the user base the MEDIA protocol is used for, according to the present invention. This GUI has already been mentioned or assumed along with the preferred embodiments of this invention, described herein, for instance, in FIG. 3 step 3 3007 , FIG. 8B messages 3 , 5 A, and 10 8016 . The user on a client platform 9015 , or 9021 in FIG. 9 is trying to reach a protected network destination 9020 . It invokes the MEDIA protocol through an interactive communication session between web server 9018 , compute server 9024 , program logic 9017 , and security and account databases 9022 and 9023 , all located on the server side, with GUI 9003 located on the client side. There are different means to implement this scheme, for example, thick or thin software client, permanently placed on a client platform, or a Java applet, loading GUI 9003 , and its respective client-side logic into a browser. The latter case in the preferred embodiment in FIG. 9 is assumed here. Also, the network, over which the communication session is established, could be either only LAN (Local Area Network), or WAN (Wide Area Network), or a combination of LAN and WAN together. In the particular embodiment in FIG. 9 , Internet 9019 is assumed as a preferred embodiment, enabling client/server dialogue through communication links 9016 .
GUI 9003 has several operation modes 9009 : login session mode 9010 , account set-up mode 9011 , user password reset mode 9012 , and server password reset mode 9013 . Login session 9010 is the default operation mode. The user enters the user name in window 9004 , the user password in window 9005 , and the server password in window 9006 . The user has a choice to enter alphanumeric characters, or their echo dots for security reasons by toggling button 9014 . The session elapsed time clock 9007 visualizes this value to the user, and signals communication session termination once the session time has expired. After the authentication credentials are all entered into 9004 , 9005 , and 9006 , the client indicates login button 9008 , which completes step 3 3007 in FIG. 3 , or message 3 in FIG. 8B . Then the other steps of the MEDIA protocol are initiated. Stoplight 9001 turns yellow, when button 9008 is indicated, signaling the MEDIA protocol is in progress for the first authentication factor (the user password) examination. Message 8 in FIG. 8B , having arrived at the client, initiates stoplight 9001 to change color from red at the beginning of the session to green, once it is checked by the client placed logic that DRK 2 delivered in the message 8 is identical to DRK 2 , delivered in message 6 .
Similarly, stoplight 9002 turns from red to the yellow color right after stoplight 9001 turned green, signaling that the MEDIA protocol is in progress for the second authentication factor (the server password) examination. Indeed, once the client received message 10 in FIG. 8B , stoplight 9002 turns green, signaling successful client/server mutual authentication, FSK exchange, and completion of the MEDIA protocol. If the client received message 5 A from the server ( FIG. 8A and FIG. 8B ), stoplight 9001 turns red, back from the yellow color, and the error message “the user password is incorrect” appears in system window 9014 , signaling the MEDIA protocol termination. Also, if the client received authentication signal “no” in message 10 from the server ( FIG. 8A and FIG. 8B ), stoplight 9002 turns red, back from the yellow color, and the error message “the server password is incorrect” appears in system window 9014 , signaling the MEDIA protocol termination.
Though, a server password unique to each user remains the preferred embodiment of this invention, various business environments, or enterprise/organization/agency IT resource configurations may require some modifications to the MEDIA protocol. The exemplary case would be when users of all computer platforms logged-in from the same server in an isolated LAN environment (or the same cluster of servers). Then the system administrator may preset the same server password at all platforms, during each platform configuration and setup on the network. This would require any user to enter only the user name, and the user password in GUI 9003 inside an enterprise, organization, or agency. Alternatively, messages 8 and 9 in the MEDIA protocol ( FIG. 9 ) could be eliminated entirely for the above case, which effectively excludes the need for server password to perform a user (a client platform) authentication and a session key exchange. However, any connection with servers and users outside the particular LAN perimeter would probably require the reinstatement of server passwords for security reasons.
While the present invention is disclosed by reference to the preferred embodiments and examples detailed above, it is to be understood that these examples are intended in an illustrative rather than in a limiting sense. It is contemplated that modifications and combinations will readily occur to those skilled in the art, which modifications and combinations will be within the spirit of the invention and the scope of the following claims. | An interactive mutual authentication protocol, which does not allow shared secrets to pass through untrusted communication media, integrates an encryption key management system into the authentication protocol. The server provides ephemeral encryption keys in response to a request during a Session Random Key (SRK) initiation interval. SRK is provided for all sessions initiated in the SRK initiation interval. A set of ephemeral intermediate Data Random Keys (DRK) is associated with each request. A message carrying the SRK is sent to the requestor. A response from the requester includes a shared parameter encrypted using the SRK verifying receipt of the SRK. After verifying receipt of the SRK at the requester, at least one message is sent by the server carrying an encrypted version of one of said set of ephemeral intermediate DRK to be accepted as an encryption key for the session. | 7 |
BACKGROUND AND SUMMARY OF THE INVENTION
In present commercial practice, when dense soils or bedrock are at moderate depths, steel "H" section piles, precast piles, or pipe piles may be driven to these soils or rock. In this way, static load capacities in excess of 80 tons are achieved. Since these piles derive their principal support at their tip, they are best categorized as "end bearing piles".
However, there are numerous conditions in which pile design permits piles to be successfully driven into granular or cohesive soils, or mixtures thereof, for the supporting of those piles. In such situations, the piles distribute their load by a combination of friction forces acting along the side of the pile and by "end bearing" forces acting beneath the tip of the pile. These piles may be steel "H" piles, precast piles, pipe piles, or mandrel-driven shell piles and are best denominated "friction piles."
Frequently a soil profile is encountered wherein unsuitable soils, i.e., those which will commpress or consolidate excessively, are underlain by bearing soils which are of only moderate or low density. While conventional "friction piles" might ultimately achieve adequate penetration for support in such soil, the depth of penetration required may be such that it can be achieved much more economically with the new and improved piles of the present invention. In accordance with the invention, a less expensive pile is provided which can be driven with greater facility through intervening layers, if any, of semi-suitable soils to the ultimate bearing layer without recourse to the time-consuming and costly special methods which heretofore might be required for state of the art types of piles.
As has been described by G. G. Meyerhof in a thesis entitled "The Ultimate Bearing Capacity of Wedge-Shaped Foundations," the ultimate bearing capacity of a foundation may be markedly increased by using a wedge of shallow depth and making the wedge of a rough surface, e.g. concrete. Numerous prior art pile devices have made use of this fundamental general "wedge" principle. The Raymond "Standard Pile," which is heavily tapered, embodies this principle. Monotube piles utilize a variety of taper configurations in conformity with this principle. Likewise, Franki piles, which are in a sense an "in situ" spread footing, nevertheless embody this wedge theory. Indeed, this general concept has also been utilized by positioning a structural, wedge-shaped mass, of larger area than the pile, at the tip (very bottom) of the pile as described in Merjan U.S. Pat. No. 3,751,931.
The present invention is directed to certain pile structures in which substantial advantages are derived from positioning a new wedge-forming structure spaced from the tip of the pile.
The principle upon which the present invention is predicated is that the frictional value between soil and soil is higher than that between steel and soil or concrete and soil. Accordingly, a soil-soil interface results in the highest value of support. This concept has been applied in a different fashion in prior art piles. For example, the concept is demonstrated by the increased capacity of corrugated shell piles versus smooth-sided pipe piles of the same length and diameter. The higher capacity of the shell results from the fact that the soil is locked in the valleys of the shell corrugations. Hence, the mode of failure is a function of the sheer strength of the soil rather than the friction between steel and soil, the former being a much higher value. Another example is found in steel "H" piles. It is well known that soil "locks" between the flanges and against the web of such piles. The locked soil results in a mode of support based on the frictional value between soil and soil.
The new and improved pile of the present invention employs a "wedge-forming element" or "wedge-former" which is spaced upwardly on the pile shaft from the tip rather than forming an actual wedge at the very tip. As a result of this unique positioning of a new "wedge-former" on the pile, during driving of the pile soil is forced to form in situ a soil wedge and to interface with other soil as the pile is driven to its ultimate depth. Specifically, soil collects under the shoulder and the tapered outer wall of the "wedge-former" and is, in effect, "locked" into the "wedge-former" (between the "wedge-former" and the shaft of the pile). The locked soil functions as a true wedge against other soil and it is this soil-soil effect which makes the new pile particularly advantageous, since, as discussed above, the frictional value between soil and soil is higher than that between steel and soil or concrete and soil. For this reason, the "soil wedge" formed in situ about the new pile provides a higher value of support at shallower driven depths than that found in earlier piles.
Because the soil wedge formed in accordance with the principles of the invention enables the pile to mobilize the soil's resistance more efficiently than known piles, the new pile need not be so massive as the Franki-type pile or the Merjan-type precast wedge tips. Hence, it lends itself to installation more economically (with conventional pile driving equipment and often to lesser depths) in a large range of soil conditions. Furthermore, the wedge-forming piles of the present invention are superior to the massive, precast concrete type of piles with integral wedges in that the new piles may more readily be driven through layers of semisuitable soils to the ultimate bearing layer without recourse to time-consuming and costly methods such as jetting or predrilling. Also, the new and improved piles of the invention avoid the uncertainties inherent in the formation of Franki-type piles, each of which is constructed according to a variety of guidelines furnished for implementation at the site. The new pile may be driven with impact pile hammers having energies in the range of approximately 15,000 to 36,000 ft.-lbs. per blow and the size of the retaining device may be readily varied to suit/load/hammer interrelationships.
The piles of the present invention may take any of several preferred forms. For instance, the "wedge-former" may be in the form of a truncated cone of precast concrete inserted onto a pipe pile and attached at an appropriate place thereon. Alternatively, the shaft and wedge-former may be integrated in the form of a unitary concrete pile. Or, in a particularly advantageous embodiment, a precast concrete point which includes an appropriately positioned wedge-former and a short section of pipe cast into its upper portion may be employed. In using this embodiment, the point is first planted into the ground. Then, the remainder of the pipe pile is connected to the section of pipe which was cast in the wedge and the pile is driven into the soil in the usual way.
It should be noted that the invention is not limited to the use of pipe piles; as will be apparent to those skilled in the art, other types of piles may be utilized. Similarly, the shape of the wedge may be varied somewhat for adaptation to different situations.
It is an object of this invention to provide a pile with improved penetration and superior support characteristics.
It is a further object of the invention to provide a pile which may be easily and economically driven into soil of inferior support quality.
For a more complete understanding of the above and other features and advantages of the invention, reference should be made to the following detailed description of preferred embodiments thereof and to the accompanying drawings.
DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a preferred embodiment of the invention including a precast concrete "wedge-former" in the form of a generally truncated cone retained on a pipe pile;
FIG. 2 is a cross-sectional view of the pile of FIG. 1, taken along the lines 2--2;
FIG. 3 is a vertical cross-sectional view of an alternate preferred embodiment of the invention including a precast pile and wedge-former;
FIG. 4 is a cross-sectional view of the pile of FIG. 3 taken along lines 4--4 thereof;
FIG. 5 is a front elevational view with parts broken away to show details of construction of another alternate preferred embodiment of the invention including a precast point attached to a pipe pile; and
FIG. 6 is a cross-sectional view of the pile of FIG. 5 taken along the lines 6--6 thereof.
FIG. 7 is a partial cross sectional view of the alternate preferred embodiment of the invention, wherein the pile cast into the concrete point is a shell pile.
FIG. 8 is a partial cross sectional view of the alternate preferred embodiment of the invention, wherein the pile cast into the concrete point is composed of precast concrete.
DETAILED DESCRIPTION OF THE INVENTION
As illustrated in FIG. 1, a first preferred embodiment of a new pile 9 comprises an elongated pile shaft in the form of cylindrical pile 10, a "wedge-former" 12 formed of a generally truncated cone of precast concrete, and a wedge-former mount 14 welded to the pile shaft. The pipe 10 is closed at its tip 15 by circular steel plate 16 welded thereto and filled with concrete 17, although in certain applications the plate 16 may be omitted for open ended driving.
The wedge-former mount 14 includes an annular retaining plate 19, vertical flanges 18, and radial webs 21 which cooperate to fasten the wedge former 14 to the pile shaft 10, as shown, in an ultimate wedge-forming position. The wedge-former 12 is fabricated from precast concrete or from any other castable material capable of withstanding the conditions encountered during driving. Concrete is generally preferred because of its rough surface. Similarly, although the shaft 10 is illustrated as a pipe, other pile shafts, such as those made of precast concrete, may advantageously be used.
The shapes of the wedge-formers of the invention may be varied depending upon the circumstances in which they are to be used. Of particular importance is that they be shaped to take advantage of the "locking" effect described earlier. In FIG. 1, the shoulder 20 and the tapered sides 22 of the wedge-former 12 function to lock the soil between the wedge-former 12 and the pile shaft, during driving. The locking effect results in the formation of a soil wedge "W" shown generally in phantom in FIG. 1, and extending from the tip 15 to the upper portions of the wedge-former 12. Because the soil wedge "W" contacts other soil, the high support value of a soil-soil interface is advantageously utilized. Furthermore, since the support value is so high, the wedge-former 12 need only be of modest size. Consequently, the new pile is less expensive to fabricate and is more easily driven through non-bearing soil layers.
The sizing of the elements of the new piles of the invention may vary in accordance with the soil environment in which they are to be used. By way of example, where nine-inch diameter, 30-40 lb./ft. load-bearing pipe pile shafts are to be used to support ultimate loads of 160 tons, the following dimensions would be appropriate for the pile of FIG. 1: the spacing "A" between the shoulder 20 and the tip 15 of the shaft 10 is 24 inches; the height "B" of the wedge-former 12 from the top 23 to the shoulder 20 is 24 inches; and the diameter of the widest portion of the wedge-former 12 is 17 inches. It will be apparent that the height of the wedge-former of the invention will be quite small relative to the depth of the bearing layer. It is not necessary that the wedge-former accompany the pile shaft for a substantial distance to realize the advantages results described herein.
In operation, the wedge-former 12 may be fastened to the pile shaft 10 at any time prior to driving. The pile 9, with the wedge-former 12 affixed thereto, is driven by conventional techniques.
An alternative embodiment of the invention is shown in FIG. 3. A precast concrete pile 24 is formed having a generally rectangular wedge-forming member 26 integral with the square shaft 28. In this form, the wedge-former is constructed as wings 27 on opposite sides of the pile shaft 28. As illustrated in FIG. 3, the wedge-former is discontinuous, i.e., it does not totally surround the pile shaft 28 of the pile 24. The thickness and the number of wings 27 is determined in accordance with the soil conditions in which the pile is to be used. The tapered base wall 30 of the wedge-former 26 functions with the lower part of the pile to cause, during driving, the formation of the soil wedge generally in the manner described hereinabove. Side wall 39 of the wedge-forming wing is substantially parallel to the pile shaft. The lower end 32 of the pile adjacent the tip 33 is tapered to facilitate penetration of the pile 24 into soil during driving. For greater strength, the concrete is provided with metal reinforcement members 34.
As noted above, the sizing of the piles of the invention may be varied, depending on the conditions in which they are to be used. By way of example, where nine-inch diameter 30-40 lb./ft. load-bearing pile shafts are to be used to support ultimate loads of 160 tons, the following dimensions may be employed for the pile of FIG. 3: the spacing "A" between the base of the wedge-forming wing 31 and the tip 33 of the pile shaft is 24 inches; the distance "B" from the top wall of the wing 35 to the base of the wing 31 is 24 inches; and the length of the widest portion of the wedge-former is 18 inches.
A particularly advantageous embodiment of the invention is depicted in the pile 36 shown in FIG. 5, which pile includes a concrete point 38 into which a short section of pipe 40 is cast. The point 38 has a central pile shaft 44 and, in its upper portions, the point includes a pair of wedge-forming wings 46 peripheral to the pile shaft. The wings include a shoulder 64 and inclined walls 58. The pile shaft extends downwards in a columnar projection 48 appropriate for inserting the point into the ground. The wings 46 function in accordance with the principles of the invention generally in the same manner as the other wedge-formers already specifically mentioned. The soil is locked beneath the shoulders 64 and inclined walls 58 against the columnar projection 48. The locked soil forms a soil wedge in accordance with the invention. The concrete may be reinforced as in the other embodiments. The columnar projection may be tapered adjacent the tip 56, as at 42, to facilitate penetration of the soil.
In operation, the point 38 is first "planted" into the ground by driving on top of the short section of pipe 40. Then, a second section of pipe 52 is attached to the short section, as by welding or with a "drive fit" 54 (also known as a mechanical connector). The entire pile assembly (pipe plus point) may then be driven into the ground using conventional driving methods.
Other types of pile shafts (other than pipes) may also be employed in association with the embodiment of FIG. 5. For instance, mandrel driven shells and precast piles may be employed in lieu of pipes FIG. 7 illustrates a pile 36A in which the short section of pile cast into the concrete point 44A is shell pile 40A. A mechanical connector 54A connects the cast section 40A of shell pile to a second section 52A of shell pile. FIG. 8 illustrates a pile 36B in which the short section of pile cast into the concrete point 44B is precast concrete 40B. A mechanical connector 54B connects the cast section 40B of precast concrete pile to a second section 52B of precast concrete pile. The wings 46A and 46B in FIGS. 7 and 8, respectively, function in accordance with the principles of the invention generally in the same manner as the other wedge formers already mentioned. The embodiments of FIGS. 7 and 8 are both used generally in the manner described for the embodiment of FIG. 5.
It should be understood that the specific forms of the invention herein illustrated and described are intended to be representative only. Changes, including but not limited to, those suggested in this specification, may be made in the illustrated embodiments without departing from the clear teachings of the disclosure. Accordingly, reference should be made to the following appended claims in determining the full scope of the invention. | A new pile is disclosed which includes a pile shaft and wedge-forming means of castable material spaced upward of the tip of the pile shaft and proximate thereto. The wedge-forming means cooperates with the portion of the pile beneath it, during driving, to cause the formation of a wedge of soil. The thus-formed soil wedge is in contact with other soil and the resulting soil-soil interface has enhanced pile supporting characteristics. | 4 |
FIELD OF THE INVENTION
The invention relates to a conveyor for handling refuse, in a street sweeping machine, carrying out refuse and dust conveying from a roadway, where said refuse and dust collection takes place, until an overlying container where the latter are stored, to be then brought to a dumping point.
DESCRIPTION OF THE PRIOR ART
Previous studies carried out by the same Applicant, described in U.S. Pat. Nos. 4,754,521 and 4,884,313 have enabled setting up of street sweeping machines internally provided with a conveyor capable of conveying refuse and the like from a roadway to an opening close to the upper end of a storage container.
Such lifting has been provided for enabling refuse unloading from a high position relative to the loading floor of said container.
This gives rise to a complete exploitation of the loading capabilities because even when the container is almost full, it is still possible to carry out loading operations.
Originally, the conveyor set up in said preceding studies has an open structure formed of shovels or blades driven by flexible support and handling members made of endless chains extending between idler members consisting of toothed wheels. This technical solution enables passage, through the conveyor itself, of a strong sucked air stream that helps in conveying refuse and dust towards the container and above all avoids spreading of dust at the roadway height.
Therefore, it is in principle superfluous to spray water over the roadway, at the refuse collecting region, in order to avoid dust spreading.
The conveyor thus made has proved to be advantageous and quite efficient.
However, it has come out that a conveyor structure based on the use of chains and toothed wheels gives rise to some noise during operation and since street sweeping machines are employed above all overnight, reduction of said noise is greatly suggested.
Chains can be replaced by belts and these have the advantage of being more silent in operation and having a lighter weight.
But, on the other hand, application of belts too creates different problems of crucial importance in the particular use in question.
In fact, shovels or blades lifting the refuse are subjected to efforts of some intensity and therefore, on the one hand, it is necessary to fix them to the belts in an efficient manner and, on the other hand, arrangement of belts capable of reliably withstanding the efforts to which they are subjected is required.
But, arrangement of effort-resistant belts necessarily involves use of belts of relatively wide dimensions. In the particular use in question belts of wide dimensions have an essential drawback: as they rest on corresponding pulleys, they give rise to wide contact regions where small debris can easily store, said debris hindering the conveyor movements until making the belts go off their races.
This problem does not exist for chains which have a reduced section and wide openings through which debris can be discharged.
It is pointed out that it is not suitable for the continuous belt structure to be modified in a substantial manner through formation of openings therein, in order to avoid weakening of them in the presence of important efforts, neither is it appropriate that the belt width should be reduced while greatly increasing thickness of same, because by so doing the belt flexibility decreases and in addition the bending efforts become of such an extent that the belt lifetime is reduced.
As regards fastening of blades to the belts, it is to note that the connecting means applied for anchoring the blades to the belts can interfere with pulleys thereby generating noise, so that it is exactly the noiselessness feature for which application of belts is desired that is eliminated.
SUMMARY OF THE INVENTION
Under this situation, the technical task underlying the present invention is to devise a new conveyor capable of eliminating the drawbacks present in known conveyors.
Within the scope of this technical task, it is an important aim of the invention to devise a noiseless and strong conveyor, which substantially cannot be clogged or damaged by the carried debris.
Another important aim is to provide a conveyor that can be also easily applied to street sweeping machines already on the market.
The technical task mentioned and the aims specified are achieved by a conveyor for handling refuse, in a street sweeping machine, comprising at least one motor, a plurality of idler members driven in rotation by said motor and defining respective rotation axes, flexible elements connected to said idler members and having an endless extension, and transport blades in engagement with said flexible elements, said flexible elements being belts having a toothed face, and said idler members being bell-shaped bodies each comprising a shaped support extending in a direction concordant with a respective rotation axis, an annular border extending radially from said shaped support, and a plurality of pins fixed with said annular border and tangentially overlying said shaped support, said shaped support supporting, in a resting condition, a portion of said pins, to be engaged in said toothed face by meshing.
BRIEF DESCRIPTION OF THE DRAWINGS
The detailed description of a preferred embodiment of a conveyor in accordance with the invention is now given hereinafter with reference to the accompanying drawings, in which:
FIG. 1 is a diagrammatic, sectional side view of the conveyor, taken as a whole;
FIG. 2 shows an enlarged portion, partly in section, of the belt of FIG. 1;
FIG. 3 is an axonometric exploded view partly in split of the structure of a bell-shaped body of the conveyor;
FIG. 4 is a partly exploded, sectional side view of the bell-shaped body of FIG. 3; and
FIG. 5 is a detailed front view of the upper portion of the conveyor.
DESCRIPTION OF THE PREFERRED EMBODIMENT
With reference to the drawings, the conveyor according to the invention is generally identified by reference numeral 1.
It is intended applied to a street sweeping machine of the type disclosed in U.S. Pat. Nos. 4,754,521 and 4,884,313 of the same Applicant.
As shown in FIG. 1, conveyor 1 extends in height from a roadway 2 to the top 3a of a container 3 in which refuse is stored, and communicates with the conveyor through an upper window 4.
Conveyor 1 has a conveying channel 5 confined by walls 5a and open at the ends, into which a sucked air stream is routed and in which there are blades 8 for refuse transport, flexible elements for supporting and moving blades 8, and idler members around which the flexible elements are disposed to form an endless configuration.
The sucked air stream is obtained by a fan, not shown, located at one end of container 3 for example, and discharging air to the outside through filters.
The flexible elements, as shown in FIG. 5, consist of two transport belts 6 parallel to and spaced apart from each other, made taut between the idler members so as to form an endless configuration, and fixed with blades 8.
Each belt 6 has a first toothed face 6a and a second smooth face 6b in contact with blades 8.
As shown in FIG. 2, each belt 6 is integral with metal elements 9 projecting from the second smooth face 6b of the belt itself.
In detail, the metal elements 9 have a first portion 9a internally of belt 6 and a second external portion 9b projecting from the second face 6b.
Preferably, the metal elements 9 are screws and the first inner portion 9a is embodied by a head 10a associated with a small plate 10b.
Blades 8 have a base 8a that by means of right-angled union pieces 8b and nuts 8c is fastened to the metal elements 9. The idle members consist of bell-shaped bodies 7, engaging the belts 6, and they are shown in an isolated position in FIGS. 3 and 4, and in an assembled position in FIGS. 1 and 5. As shown in the last-mentioned figures the bell-shaped bodies 7 have a rotation axis 11a along which a shaft 11 is disposed and said shaped bodies do not directly engage said shaft 11, as they are provided with a central hole 12 of greater diameter than the shaft 11. In fact, a flange 13 fixed in rotation with shaft 11 is interposed between each bell-shaped body 7 and the related shaft 11.
Four bell-shaped bodies 7 and two shafts 11 defining two axes 11a at the upper and lower ends of the conveying channel 5 are present as a whole in the conveyor.
In addition, each bell-shaped body 7 is divided into two halves 7a susceptible of mating at a split 14 lying in a plane passing through the rotation axis 11a. Halves 7a are screwed down in a removable manner to flange 13 by screw connections 15, shown in FIG. 5.
Still with reference to FIG. 5 it is pointed out that at least part of the bell-shaped bodies 7 is powered, due to the presence of a motor 16, for example.
As shown in FIGS. 3 and 4, the bell-shaped bodies 7 are embodied by a shaped support 17 extending at least partly parallel to axis 11a, by an annular border 18 radially emerging from one end of the shaped support 17, and by a plurality of pins 19 fixed the annular border 18 and projecting in cantilevered fashion from the latter, in a direction concordant with the shaped support 17 and parallelly of axis 11a.
Practically, pins 19 tangentially surround the shaped support 17, the latter supporting a pin portion in a mere resting condition.
In detail, pins 19 are of cylindrical form and welded at one end thereof to the annular border 18, where circumferentially spaced circular positioning holes 18a are provided which are exactly shaped to size for mating with pins 19.
The shaped support 17 is formed of a tubular protuberance 20 and a disk-like plate 21.
The tubular protuberance 20 extends from the annular border 18 in a direction parallel to pins 19 and to axis 11a over a Length corresponding to about half the length of the pins or smaller than said length, whereas the disk-like plate 21 is parallel to the annular border 18 and perpendicular to the rotation axis 11a and extends from the annular protuberance 20 end opposite to the end engaged by the annular border 18. In addition, the disk-like plate 21 extends in a centripetal direction, until it forms said central hole 12 and is directly connected to said flange 13.
It is also to point out that in the annular border 18 the circular positioning holes 18a terminate tangentially to or flush with the tubular protuberance 20, so that the cylindrical pins 19 are in contact with said tubular protuberance 20 at a portion of a generating line thereof. FIGS. 3 and 4 show that preferably the annular border 18 and tubular protuberance 20 are concerned with through cuts 22 disposed radially of the rotation axis 11a. The through cuts 22 are at the sides of each positioning hole 18a and each pin 19, and divide the annular border 18 and tubular protuberance 20 into segments.
As shown in FIG. 5, the bell-shaped bodies 7 located at the upper part of the conveying channel 5 can be positioned in a vertical direction, so as to enable tensioning of belts 6. Positioning of shaft 11, the related bell-shaped bodies 7 and motor 16 is made possible by engagement of elements 7, 11, 16 with movable supporting plates 23 adapted to cover openings 24 formed in the walls 5a of the conveying channel 5.
The supporting plates 23 are slidably engaged on walls 5a in any suitable manner and also displacement of said supporting plates can be obtained by any tensioning device.
Belts 6 must then keep a correct position in a direction parallel to axes 11a and FIG. 5 shows that a correct position is obtained by virtue of blades 8 connecting belts 6 to each other, and by virtue of the annular borders 18 being in contact with the side edges of belts 6 and projecting externally of blades 8. In fact, each annular border 18 comprises a rim 18b extending in a radial direction beyond the positioning holes 18a.
Practically, due to rim 18b and to the fact that at each axis 11a two bell-shaped bodies 7 mounted in alignment and capable of being overturned in mirror image relationship are provided, the annular borders 18 emerge from an edge of belts 7 to form a lateral holding border of the belts themselves. Operation of the conveyor is as follows.
Belts 6 from a structural point of view appear already arranged for engagement with blades 8, in that the metal elements 9 project from a face thereof. Said metal elements are anchored in a very efficient manner in that they have their first portion 9a completely buried in the belts and locked therein.
The first toothed face 6a is thus completely free from metal elements and in any case from elements projecting in a very localized manner and can ensure a noiseless contact with the bell-shaped body 7.
The bell-shaped bodies 7 have pins of wide sizes, but debris storage is in any case avoided due to the circular section of pins 19 eliminating any flat rest surface thereon, and to the position in cantilevered fashion of the pins themselves which are substantially free because they are only marginally and over a reduced portion thereof in contact with the tubular protuberance 20 of the shaped support 17. In addition, since said support is provided with through cuts 22, its presence does not give rise to debris storage regions.
Although pins are of the cantilevered type and substantially free, strength of the bell-shaped bodies 7 is ensured by partial resting of pins 19 on the shaped support 17. In addition, fastening of said pins 19 in a correct and precise location is very facilitated by arrangement of the positioning holes 18a.
Finally, the bell-shaped bodies 7 can be immediately fitted on flanges 13 and disassembled therefrom, due to their division into two halves 7a. Therefore it is not necessary to axially slip the shaft 11 off for fitting of said bell-shaped bodies.
The invention achieves important advantages.
In fact, the described conveyor reaches the advantages of being noiseless in operation, light in weight and cheap. It is also reliable, of strong structure, can be easily assembled and above all it does not substantially suffer from clogging problems due to debris building-up, which problems are crucial in this type of application. | The invention is directed to a conveyor operated by idler members driven in rotation by a motor (16) which includes a pair of spaced apart flexible elements connected to the idler member and having an endless extension. Refuse transporting blades (8) are in engagement with the pair of flexible elements. The flexible elements are belts (6) having a toothed face (6a), and the idler member are bell-shaped bodies (7) each having a shaped support (17) parallel to a respective rotation axis (11a), an annular border (18) extending radially from the shaped support (17), and circumferentially spaced pins (19) for meshing with the toothed face (6a) of the belts (6). The pins (19) are fixed to the annular border (18) and tangentially overlie the shaped support (17) which supports a portion of the pins (19) in a resting condition. | 1 |
CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 60/613,150 entitled “Point Anchor Resin Bolt” filed Sep. 24, 2004.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a mine roof bolt anchored in a bore hole by mechanical anchoring and resin bonding, and more particularly to a mine roof bolt bearing an expansion assembly and a segmented resin compression layer that exerts a compressive force on resin within a bore hole.
2. Prior Art
The roof of a mine conventionally is supported by tensioning the roof with 4 to 6 feet long steel bolts inserted into bore holes drilled in the mine roof that reinforce the unsupported rock formation above the mine roof. The end of the mine roof bolt may be anchored mechanically to the rock formation by engagement of an expansion assembly on the end of the mine roof bolt with the rock formation. Alternatively, the mine roof bolt may be adhesively bonded to the rock formation with a resin bonding material inserted into the bore hole. Alternatively, a combination of mechanical anchoring and resin bonding can be employed by using both an expansion assembly and resin bonding material.
A mechanically anchored mine roof bolt typically includes an expansion assembly threaded onto one end of the bolt shaft and a drive head for rotating the bolt. A mine roof plate is positioned between the drive head and the mine roof surface. The expansion assembly generally includes a multi-prong shell supported by a threaded ring and a plug threaded onto the end of the bolt. When the prongs of the shell engage with rock surrounding a bore hole, and the bolt is rotated about its longitudinal axis, the plug threads downwardly on the shaft to expand the shell into tight engagement with the rock thereby placing the bolt in tension between the expansion assembly and the mine roof surface.
When resin bonding material is used, it penetrates the surrounding rock formation to adhesively unite the rock strata and to firmly hold the roof bolt within the bore hole. Resin is typically inserted into the mine roof bore hole in the form of a two component plastic cartridge having one component containing a curable resin composition and another component containing a curing agent (catalyst). The two component resin cartridge is inserted into the blind end of the bore hole and the mine roof bolt is inserted into the bore hole such that the end of the mine roof bolt ruptures the two component resin cartridge. Upon rotation of the mine roof bolt about its longitudinal axis, the compartments within the resin cartridge are shredded and the components are mixed. The resin mixture fills the annular area between the bore hole wall and the shaft of the mine roof bolt. The mixed resin cures and binds the mine roof bolt to the surrounding rock. The typical diameter of a mine roof bore hole is one inch. Mine roof bolts anchored with resin bonding are often ¾ inch in diameter, and more recently ⅝ inch in diameter. The mine roof bolt is generally centered within the bore hole creating a circular annulus that becomes filled with bonding resin. The larger diameter bolts (¾ inch) offer performance advantages over ⅝ inch bolts in that the annulus provided between the bore hole wall and a ¾ inch bolt is smaller than that of smaller diameter bolts. A smaller annulus provided between the bolt and the bore hole wall improves mixing of the resin and catalyst in the annulus. In addition, when the resin cartridge is shredded upon insertion of the mine roof bolt and rotation thereof in an annulus larger than ⅛ inch (as for mine roof bolts having less than ¾ inch diameter installed in one inch bore holes), the shredded cartridge can interfere with the resin and catalyst mixing. Poor mixing results in an inferior cured resin and results in poor bond strength between the bolt and bore hole wall. This phenomenon of “glove fingering” occurs when the plastic film that forms the cartridge lodges in the bore hole proximate the surrounding rock thereby interrupting the mechanical interlock desired between the resin and bore hole wall. In addition, the larger annulus created by using a ⅝ inch bolt in a one inch bore hole requires more resin to bond the bolt to the rock than does a larger diameter bolt, thereby adding to the cost of installing a smaller diameter bolt. While one solution would be to proportionally reduce the size of the bore hole to less than one inch, this is not practicable. The mine roof drilling equipment in use is conventionally produced for drilling one inch bore holes. Moreover, there are significant technical difficulties in drilling small diameter bore holes in mine roofs.
Despite these drawbacks of using mine roof bolts having a diameter of less than ¾ inch, the popularity of smaller diameter mine roof bolts is increasing. A ⅝ inch bolt is lighter and easier to use than a ¾ inch bolt and can be produced at lower cost. One solution for overcoming the need for extra resin and avoiding the glove fingering problem of smaller diameter bolts installed in one inch bore holes has been provided in a proposed mining bolt which includes an elongated rod that forms the main structure of the mine roof bolt as disclosed in U.S. Patent Application Publication No. 2005/0134104. A portion of the rod in between a drive head and the end of the bolt is coated with a layer of material having a lower specific gravity than the rod, such as a polymer. The polymeric coating layer may have external texturing which can help with mixing of resin in the mine roof bore hole. The coating on the mine roof bolt also helps to fill some of the annulus at a minimal increase in weight to the bolt and minimizes the amount of resin that is required for bonding the bolt to rock strata. This coated mine roof bolt can be produced from a ⅝ inch metal rod with a polymeric coating layer about 1/16 inch thick. The coated mine roof bolt uses only resin bonding to anchor the mine roof bolt to a rock formation.
However, the combination of both mechanical anchoring and resin bonding of mine roof bolts has been found to provide superior mine roof control. A mine roof bolt having an expansion assembly with expansion shell and plug is held against the surface of a mine roof by a plate. Rotation of the bolt mixes the resin components and expands the expansion shell. The resin mixture surrounds the expansion assembly and several feet of the mine roof bolt. Upon hardening of the resin mixture, the bolt is anchored to the rock strata by the resin and the expansion assembly. In some mine roof bolts that are anchored by a combination of resin bonding and expansion assembly anchoring, a device is used to delay relative rotation between the expansion assembly and the mine roof bolt until the resin is hardened so that the bolt can be tensioned after the resin begins to harden. An anti-rotation device prevents relative rotation between the plug of an expansion assembly and the bolt so that the plug does not thread down the bolt during mixing of the resin components. One suitable anti-rotation device is a shear pin extending through the plug. The resin components are thoroughly mixed before the shell of the expansion assembly is expanded. The end of the bolt abuts the pin to prevent initial downward movement of the plug on the bolt during rotation of the bolt to effect mixing of the resin components. Once the resin begins to set, the force on the shear pin exceeds its strength and continued rotation of the bolt shears through the pin and allows the plug to advance downwardly on the bolt to expand the shell of the expansion assembly outwardly to grip the bore hole wall.
For mine roof bolts that are anchored using a combination of a mechanical anchor and resin bonding and for coated mining bolts that are anchored with resin, the resin is desirably maintained in an upper region of the bore hole. However, retention of the resin adjacent the upper portion of the mine roof bolt is problematic. One solution has been to include a resin retaining washer at a position intermediate the end of the mine roof bolt and the mine roof for restricting the annular area in which the resin may flow. The upward thrust of a mine roof bolt bearing a resin retaining washer can exert a hydraulic force on the resin to confine it within the restricted annular area at the end of the mine roof bolt and forcibly drive the resin into the cracks and crevices on the inside of the bore hole and into the surrounding rock formation to more solidly lock the mine roof bolt within the rock formation. However, such resin retaining washers are limited in their ability to block resin from flowing downwardly along the bolt. While a resin retaining washer can withstand the hydraulic pressure created when the mine roof bolt shreds the resin capsule, nothing on the mine roof bolt urges the resin back upwardly into the bore hole.
Accordingly, a need remains for a mine roof bolt which utilizes a combination of mechanical anchoring and resin bonding to anchor the mine roof bolt in a bore hole (particularly for a small diameter mine roof bolt such as ⅝ inch) where the resin mixing and distribution is controlled by the bolt.
SUMMARY OF THE INVENTION
This need is met by the mine roof bolt of the present invention which includes an elongated rod having a threaded end and a drive end. An expansion assembly composed of an expansion shell and plug are threaded onto the threaded end. A segmented resin compression layer covers a portion of the elongated rod between the threaded end and drive end. The segmented layer includes a plurality of tapered segments with each segment having a first portion that is thicker than a second portion. Each segment also includes an exterior thread that is discontinuous with the thread of an adjacent segment. The surface of each segment may be textured such as by a plurality of ridges extending between the first and second portions. The segmented layer may also include a tapered portion that extends and tapers from a first portion of a terminal segment in closest proximity to the expansion anchor to a position spaced therefrom. The mine roof bolt may further include a resin retaining ring adjacent the end of the segmented layer that is closest to the drive end. The elongated member may be a smooth bar or a textured bar such as rebar. The segmented resin compression layer may be produced from a polymeric material.
When the mine roof bolt of the present invention is installed in the mine roof bore hole, a frangible curable resin cartridge is inserted into the bore hole. The mine roof bolt is inserted into the bore hole and ruptures the resin cartridge. The mine roof bolt is rotated along its longitudinal axis such that the resin compression layer contributes to mixing the contents of the resin cartridge and compresses the resin between the mine roof bolt and the bore hole wall. Rotation of the bolt causes the expansion assembly to engage with the bore hole wall. The expansion assembly may include a delay mechanism for delaying the time at which the expansion assembly expands to engage with the bore hole wall. The resin compression layer includes a plurality of tapered segments, whereby a thicker portion of each segment compresses the resin within the bore hole. In addition, the surface of each segment includes a spiral thread that urges the resin toward the threaded end upon rotation of the mine roof bolt.
The mine roof bolt of the present invention may be produced by providing an elongated rod and applying a segmented layer to the rod intermediate the ends thereof. An expansion assembly is threaded onto one end and a drive head is attached to the other end of the rod. The segmented layer may be polymeric and may be applied to the rod by injection molding.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of a mine roof bolt having a segmented resin compression layer of the present invention, an expansion assembly, a resin retaining ring and a drive head;
FIG. 2 is a side elevational view of the mine roof bolt of FIG. 1 , from an opposing side thereof;
FIG. 3 is a cross section of the mine roof bolt of FIG. 1 taken along lines 3 — 3 ;
FIG. 4 is a plan view of the resin retaining ring shown in FIG. 1 ;
FIG. 5 is a side elevational view of another embodiment of the mine roof bolt of the present invention wherein the segmented resin compression layer includes a terminal tapered portion;
FIG. 6 is a side elevation partially in section of one step of the method of installing the mine roof bolt of the present invention, illustrating the resin cartridge in position at the end of the bore hole for rupture by the expansion assembly;
FIG. 7 is a view similar to FIG. 6 , illustrating mixing of the components of the ruptured cartridge by rotation of the bolt;
FIG. 8 is a graph of the deflection of mine roof bolts versus load for the mine roof bolt of the present invention conducted in a laboratory; and
FIG. 9 is a graph similar to FIG. 8 for a mine test.
DETAILED DESCRIPTION OF THE INVENTION
A complete understanding of the present invention will be obtained from the following description taken in connection with the accompanying drawing figures, wherein like reference characters identify like parts throughout.
For the purposes of the description hereinafter, the terms “upper”, “lower”, “right”, “left”, “vertical”, “horizontal”, “top”, “bottom” and derivatives thereof relate to the invention as it is oriented in the drawing figures. However, it is to be understood that the invention may assume alternative variations and step sequences, except where expressly specified to the contrary. It is also to be understood that the specific devices and processes illustrated in the attached drawings and described in the following specification are exemplary embodiments of the invention. Specific dimensions and other physical characteristics related to the embodiments disclosed herein are not considered to be limiting.
Referring to the drawings and particularly to FIGS. 1–3 , there is illustrated a mine roof bolt 10 for securing in a bore hole 12 drilled in a rock formation 14 to support the rock formation 14 that overlies an underground excavation such as a mine passageway or the like. The bore hole 12 is drilled to a pre-selected depth into the rock formation 14 as determined by the load bearing properties to be provided by the mine roof bolt 10 .
The bolt 10 includes an elongated rod 16 having a threaded end 18 for positioning in the upper blind end 20 of the bore hole 12 and a drive end 22 having a drive head 24 that extends into the mine passageway from the open end of the bore hole 12 . A roof or bearing plate 26 is retained by the drive head 24 on the end 22 of the bolt 10 . The drive head 24 generally includes a shoulder 28 and a plurality of drive faces 30 . The rod 16 , roof plate 26 and drive head 24 typically are produced from steel. An expansion assembly 32 is threaded onto the threaded end 18 of the bolt 10 . The expansion assembly 32 shown in FIGS. 1–3 includes an expansion shell 34 having a base portion 36 in the configuration of a ring or collar to which are integrally attached a plurality of upwardly extending expansion leaves 38 that are spaced from one another and having free ends. A tapered plug 40 is threaded on the rod 16 into the inside of the expansion shell 34 . The tapered plug 40 is configured to move downwardly toward the base 36 of the expansion shell 34 upon rotation of the bolt 10 while the expansion leaves 38 bend outwardly into gripping engagement with the rock formation 14 . Other expansion shell assemblies that may be used in the present invention include bail type shells in which two expansion leaves are supported by a bail that extends over the end of the mine roof bolt and prevents expansion of the leaves from moving axially relative to the bolt until desired. In addition, the expansion assembly 32 may include a stop mechanism (not shown) such as disclosed in U.S. Pat. No. 4,419,805 to Calandara, Jr., incorporated herein by reference. An expansion shell assembly having a stop device prevents expansion of the shell assembly during the stage of mixing resin with the bolt. When the torque applied to the bolt exceeds a pre-determined torque as determined by the time for mixing the bonding material, the stop device fractures and the expansion shell assembly is then free to expand into gripping engagement with the wall of the bore hole as the plug is threaded downwardly on the bolt. In any of these expansion shell assemblies, the bolt 10 is both mechanically anchored and adhesively bonded in the bore hole to prevent slippage of the expansion assembly 32 so that the bolt remains tensioned to support the rock formation 14 .
A portion of the elongated rod 16 between the threaded end 18 and the drive end 22 is covered with a resin compression layer 42 . The elongated rod 16 may be a smooth rod or a textured rod such as rebar, with a smooth rod being shown in the drawings herein. In one embodiment of the invention, the resin compression layer 42 extends from a position about one inch from the lower end of the expansion assembly 32 for about sixteen to twenty inches down the length of a four foot mine roof bolt 10 . Other lengths of the resin compression layer 42 may be selected relative to the length of the bolt 10 , depending on the roof anchoring needs.
The resin compression layer 42 includes a plurality of tapered segments 44 . Each tapered segment has a first portion 46 that is thicker than a second portion 48 as shown in FIG. 3 . The tapered segments 44 create a mechanical wedging force when load is applied to the bolt 10 . The surface of segment 44 includes a spiral thread 50 , each spiral thread 50 of a segment 44 being discontinuous with the thread 50 of an adjacent segment 44 . The spiral threads 50 may be ribbed as shown ( FIG. 3 ) or may be smooth. The spiral threads 50 of the tapered segments 44 urge resin upwardly into the bore hole 12 upon rotation of the bolt 10 during mixing of resin. The tapered segments 44 may also include texturing such as a plurality of ridges 52 that extend between the first and second portions 46 , 48 . The texturing further assists in mixing and distributing the resin around the mine roof bolt 10 .
Referring to FIG. 5 , a resin retaining ring 54 may also be used for maintaining resin within the annulus between the bolt and the bore hole in the location of the resin compression layer 42 . The resin retaining ring 54 may be generally circular shaped with recessed portions 56 that allow for adjustment of the diameter of the ring 54 when compressed within the bore hole 12 .
In another embodiment of the invention shown in FIG. 5 , a mine roof bolt 110 includes a resin compression layer 142 having a plurality of tapered segments 44 and a terminal tapered portion 144 that extends from a terminal segment 44 a to a position spaced apart from the threaded end 18 . This tapered portion 144 smoothes the transition between the tapered segments 44 and the elongated rod 16 and eases insertion of the bolt 110 into a bore hole. Hereinafter, all references to the mine roof bolt 10 are applicable to mine roof bolt 110 .
The mine roof bolt 10 of the present invention may be produced by coating the elongated rod 16 with a flowable polymer so that the coating has a thickness such as of about at least 1 mm. The polymer is allowed to solidify on the elongated rod 16 and texturing is applied to the exterior of the polymer to form the spiral threads 50 and ridges 52 . The coating step may be performed by dip coating, injection molding and/or hot forging of the polymer resulting in an outer layer of a low density hard coating of the resin compression layer 42 on an inner portion of higher density material (e.g., steel) of the elongated rod 16 . Because the resin compression layer 42 is typically formed from a polymer, the low density hard coating that is applied as a resin compression layer 42 increases the overall diameter of a portion of the bolt 10 with a minimal increase in weight. Hence, while realizing the weight advantages of polymers as compared to metals used in an elongated rod 16 , such a composite bolt 10 can be advantageously sized to provide improved mixing of resin by creating a smaller annulus between the bolt in the location of the resin compression layer 42 and the rock 14 surrounding the bore hole 12 . Likewise, with reduced annulus dimensions, less resin is required for bonding the bolt 10 within the bore hole 12 with concomitant reduction in the size and quantity of shredded resin packaging film that remains after mixing.
In one embodiment of the invention, the elongated rod 16 is a smooth rod and the polymer coating is produced by molding to create the ridges 52 and spiral threads 50 . Typically, the thickness of the coating is sufficient to minimize the annulus between the resin compression layer and the bore hole wall at less than ⅛ inch or less than 1/16 inch. This reduces the overall weight of the mine roof bolt 10 , particularly if the coating is a polymer of low density, such as about 2.0 g/ml or less.
Referring to FIGS. 6 and 7 , in accordance with the present invention, the mine roof bolt 10 may be installed in a mine roof to provide support to the rock formation 14 . In one embodiment of the method of supporting a mine roof, the mine roof bolt 10 is installed by inserting a frangible resin cartridge 58 into a bore hole 12 and inserting the mine roof bolt 10 into the bore hole 12 . The mine roof bolt 10 includes an elongated rod 16 having a threaded end 18 onto which an expansion assembly 32 is threaded and a drive end 22 extending out of the bore hole 12 . A resin compression layer 42 covers a portion of elongated rod 16 intermediate the drive end 22 and expansion assembly 32 . When the threaded end 18 of the mine roof bolt 10 contacts the resin cartridge 58 , the cartridge 58 ruptures releasing a curable resin 60 . The mine roof bolt 10 is rotated about its longitudinal axis so that the expansion assembly 32 , resin compression layer 42 and any exposed portion of elongated rod 16 mixes the contents of the resin cartridge 58 . The tapered segments 44 of the resin compression layer 42 compress the resin 60 between the exterior of the mine roof bolt 10 and the bore hole wall. The expansion assembly 32 may include a stop mechanism that resists relative rotation between the bolt 10 and the plug 40 until a torque in excess of a predetermined torque is applied to the drive end 22 of the bolt 10 . At this torque, the resistance offered by the curing resin 60 to rotation of the plug 40 fractures the stop mechanism. When the torque for breaking the stop mechanism is reached, resin mixing is complete and the plug 40 travels downwardly into the expansion shell 34 . In this manner, expansion of the shell 34 is delayed until the resin 60 is mixed, but not after the resin 60 completely rigidifies in the bore hole 12 . The stop mechanism includes any suitable device that restrains axial movement of the plug 40 on the bolt 10 beyond a pre-selected point on the threaded end 18 of the bolt 10 , such as a breakable obstruction member (e.g., a shear pin) suitably retained within the plug 40 .
The resin compression layer 42 serves several functions during installation of the mine roof bolt 10 and after it is installed in a mine roof. As the bolt 10 is rotated about its longitudinal axis, the spiral threads 50 on the resin compression layer urge resin upwardly toward the blind end 20 of the bore hole 12 . Retention of resin 60 at the blind end 20 of the bore hole 12 is desired to ensure good bonding between the mine roof bolt 10 and the surrounding rock 14 and to concentrate the anchoring function at the threaded end 18 of the bolt 10 . Sufficient resin is required in the annulus between the mine roof bolt 10 and the bore hole wall to completely fill the annulus and allow for some of the resin 60 to fill cracks and crevices in the rock 14 to enhance the interlock between the rock 14 and the mine roof bolt 10 . In addition, such bolts that are anchored by a combination of mechanical components (expansion shells) and resin bonding, the location of the mechanical/resin anchor spaced apart from the mine roof surface creates a “point anchor” that permits tensioning of the bolt between the mechanical/resin point anchor and the mine roof surface. Retention of the resin at the upper end of the bolt is required to achieve a point anchor system that is tensionable.
The resin compression layer 42 also serves to mix the resin 58 . The spiral threads 50 and the ridges 52 provide mixing surfaces to enhance mixing of the curable resin 58 . The segmented arrangement of the resin compression layer 42 also provides surface disruptions that enhance mixing.
Upon application of load to the mine roof bolt, the tapered surfaces of the segments 44 create mechanical wedging forces that resist pull out of the bolt 10 from the bore holes. The thicker portion (upper end) 46 of each segment 44 compresses the resin 58 towards the bore hole wall.
In certain applications, the mine roof bolt 110 shown in FIG. 5 having a resin compression layer 142 with a terminal tapered portion 144 improves installation in a mine roof bore hole 12 . The terminal tapered portion 144 provides a transition surface from the rod 16 to the resin compression layer 142 , which eases insertion into a bore hole 12 .
Experiments were conducted to determine the performance of the mine roof bolts of the present invention.
A laboratory pull test was conducted on bolts produced according to the present invention. Four bolts produced according to the present invention were used. For two of the bolts, prior to coating with the resin compression layer, the elongated rod was wiped with a cloth to remove contaminants such as oil, dirt or grease. The other two rods were not cleaned prior to coating. The bolts were installed in threaded steel bore holes and resin bonded using Insta'l 2 resin cartridges available from Jennmar Corporation of Pittsburgh, Pa. (two minute gel time, 1¼ inch diameter×13 inch long) in a 22 inch bore hole. Bolting machine thrust was set at 3000 pounds. After curing of the resin, the ends of the bolts bearing the expansion assembly were cut off and the remaining portions of the mine roof bolt were tested in a hydraulic pull apparatus to measure deflection as function of load. The test was designed to determine the load that is required to debond the resin compression layer from the elongated rod. The results of the pull test are shown in FIG. 8 . Bolts A and B (cleaned bolts) exhibited respective maximum loads of 13,000 pounds and 13,500 pounds at an average unit strength of 806 pounds per inch. Bolts C and D (uncleaned) exhibited maximum loads of 12,000 pounds and 10,500 pounds, respectively, with an average unit strength of 683 pounds per inch.
The mine roof bolts of the present invention were tested for deflection in the roof of a coal mine along with bolts of the prior art. Two bolts of the present invention included a tapered portion at the end of the resin compression layer and two bolts had no tapered portion. Three bolts of the prior art (Insta'l 2 bolts available from Jennmar Corporation) were tested for comparison.
The resin used for bonding all bolts was H2 resin with one minute gel time. The mine roof bolts of the present invention were installed with resin 1¼ inch diameter×14 inch long cartridges and the prior art bolts were installed with 1¼ inch×20 inch resin cartridges. Less rotation was required to install the bolts of the present invention than the prior art bolts. The bolts having a tapered end portion were easier to insert into the bore holes than the bolts not having the tapered portion. The results of a pull test are shown in FIG. 9 . For loads up to about 10–11 tons, the bolts of the present invention (“A” no tapered portion, “B” with tapered portion and “Average” thereof) and prior art bolts exhibited similar deflection. At higher loads, greater deflection was exhibited by the bolts of the present invention, which may have been due to debonding of the resin compression layer from the elongated rod.
While the present invention has been described with reference to particular embodiments of a mine roof bolt and methods associated therewith, those skilled in the art may make modifications and alterations to the present invention without departing from the spirit and scope of the invention. Accordingly, the foregoing detailed description is intended to be illustrative rather than restrictive. The invention is defined by the appended claims, and all changes to the invention that fall within the meaning and the range of equivalency of the claims are embraced within their scope. | A resin bonded mine roof bolt having an elongated rod with a drive head at one end and an expansion anchor threaded onto the other end. A segmented resin compression layer covers a portion of the rod below the expansion anchor. When installed in a mine roof bore hole with curable resin, the resin compression layer mixes the resin and partially fills the bore hole to minimize the amount of resin needed to anchor the bolt. Individual segments of the layer are tapered to create a wedging force on resin with the bore hole. The expansion anchor is expandable upon initial hardening of the resin to tension the bolt. | 4 |
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